CN106248674A - A kind of edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae - Google Patents

A kind of edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae Download PDF

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CN106248674A
CN106248674A CN201610647315.4A CN201610647315A CN106248674A CN 106248674 A CN106248674 A CN 106248674A CN 201610647315 A CN201610647315 A CN 201610647315A CN 106248674 A CN106248674 A CN 106248674A
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sample
rice
edible
semen oryzae
quality
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许立
闵捷
胡贤巧
于永红
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China National Rice Research Institute
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China National Rice Research Institute
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103—Atomic absorption analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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Abstract

The present invention relates to a kind of edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae.Currently there are no a kind of quality of rice stage division, set up a kind of perfect quality of rice classification (evaluation) method to instruct the production of China's rice product, consumption the most necessary.Present invention is characterized in that the step of described method is as follows: (1) takes rice sample, the chalkiness degree of detection rice sample；(2) rice sample is taken, the persticide residue in detection rice sample；(3) rice sample is taken, the heavy metal cadmium content in detection rice sample；(4) chalkiness degree, persticide residue and the heavy metal cadmium content obtained according to detection, carries out quality grading to rice.The detection speed of the present invention is fast, accuracy is high, and reagent saves, environmentally friendly, also have stability and reproducible, and Producer can fix a price by credit rating, the optional purchase of consumer, can really embody high quality and favourable price.

Description

A kind of edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae
Technical field
The present invention relates to a kind of edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae, both may be used for edible Semen Oryzae is entered Row quality grading, may be used for again edible Semen oryzae sativae is carried out quality grading.
Background technology
Oryza sativa L. is the topmost cereal crops of China, and its total output accounts for the 40% of total output of grain, and the whole nation has more than 60% Population with rice as staple food, the product quality of rice is healthy closely bound up with our people's.Along with social economy is sent out Exhibition improves constantly with living standards of the people, and people are more and more higher to the requirement of rice product quality, safe, nice, good-looking It it is modern people's new demand to rice product quality.Therefore, a kind of perfect quality of rice classification (evaluation) method is set up Instruct the production of China's rice product, consumption the most necessary.Although also there being now the side of detection/prediction rice safe mass Method, if publication date is on 03 19th, 2014, in the Chinese patent of Publication No. CN103645201A, discloses a kind of based on X Ray fluorescence quickly detects the method for heavy metal cadmium in rice, and and for example publication date is on 06 10th, 2015, Publication No. In the Chinese patent of CN104686267A, disclose a kind of method of heavy metal cadmium content in early prediction rice, but now Also there is no a kind of edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae.
Summary of the invention
It is an object of the invention to overcome above-mentioned deficiency present in prior art, and provide a kind of detection speed fast, accurate Exactness is high, and reagent saves, environmentally friendly, also have stability and reproducible, and Producer can be fixed a price by credit rating, and consumer can Select to buy, can really embody edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae of high quality and favourable price.
The present invention solves the problems referred to above and be the technical scheme is that this edible Semen Oryzae and the quality grading side of edible Semen oryzae sativae The feature of method is: the step of described method is as follows:
(1) rice sample is taken, the chalkiness degree of detection rice sample；
(2) rice sample is taken, the persticide residue in detection rice sample；
(3) rice sample is taken, the heavy metal cadmium content in detection rice sample；
(4) chalkiness degree, persticide residue and the heavy metal cadmium content obtained according to detection, carries out quality grading to rice.
As preferably, the method for the invention also comprises the steps: to take rice sample, the edible product of detection rice sample Matter；Then chalkiness degree, edible quality, persticide residue and the heavy metal cadmium content obtained according to detection, carries out quality to rice Classification.
As preferably, in step of the present invention (1), the determination step of chalkiness degree is as follows: divide with riffle sampler that to take 10g～35g big Rice sample, is placed in rice sample on scanner glass plate, and weak vibrations causes to scatter between the grain of rice and the most overlapping, scanned sample, Obtain rice Sample Image, automated randomized from scanning figure choose no less than 100 complete polished rice Sample Images, be aided with and manually pick Except staying skin or embryo to be judged to the grain of rice image that chalk is white rice sample by mistake, finally calculate chalkiness degree.
As preferably, the step of the edible quality that the present invention detects rice sample is as follows:
Preparing of low-volume samples rice is as follows:
Claim sample: weigh every part of 10g sample in dewatering screen；
Washing rice: be placed in basin by dewatering screen, rapidly join 150mL tap water, stirring 10 circle, stirs counterclockwise the most clockwise Mixing 10 circles, quick water change repeats aforesaid operations once；Again with 150mL aquae destillata drip washing 1 time, the most remaining water of drip, people numbers accordingly Steamed rice ware in；Washing meter time controls at 3min-5min；
Soak: Semen Oryzae adds 1.6 times that the distilled water yield is sample size, and Semen oryzae sativae adds 1.3 times that the distilled water yield is sample size；Soak Water temperature about 25 DEG C, soak time 30min；
Steaming and decocting: add appropriate water in steamer, be heated to boiling, take off pot cover, then the steamed rice ware holding sample is added a cover Place on steaming tray, cover pot cover, continue heating and start timing, steaming and decocting 40min, stop heating, vexed meal 20min, judge while hot；
Preparing of a large amount of sample rice is as follows:
Claim sample: weigh every part of 500g；
Wash rice: the 500g sample weighed is put into dewatering screen, is placed in basin by dewatering screen, rapidly join 1500ml from the beginning Water, the most clockwise stirring 10 circle, counterclockwise stirring 10 circle, quick water change repeats aforesaid operations once；Use 1500mL distilled again Water wash 1 time, the most remaining water of drip, in the directly-heated type electric cooker that people numbers accordingly；Washing meter time controls at 3-5min；
Steaming and decocting: electric cooker switches on power beginning cooking rice, must not open pot cover in digestion process；The switch of electric cooker After tripping, more vexed 20min processed；
Stirring rice: spoon of having a meal stirs well-done rice, first loosens from the periphery of pot, makes rice separate with pot wall, then By each parallel sliding of both direction 2 times anyhow, then stir up and down with chopsticks 4 times, after making unnecessary moisture evaporation, cover pot Lid, more vexed 10min；
50g sample rice is loosely contained in little bowl, everyone 1 part, then tips upside down on positions different on white porcelain service plate Put, in bacterium taper, judge while hot.
As preferably, in step of the present invention (2), use organophosphor in gas chromatography determination rice sample, organochlorine and Determining pyrethroid pesticide residues, the detecting step of persticide residue is as follows: organophosphor, organochlorine and pyrethrin pesticide in rice sample Through acetonitrile extraction, extracting solution is saltoutd through magnesium sulfate, after PSA dispersive solid-phase extraction purifies, detects with FPD after air inlet chromatography Device detects, and carries out qualitative according to retention time, area quantified by external standard method；Or, organochlorine and pyrethrin pesticide in rice sample Through acetonitrile extraction, extracting solution is saltoutd through magnesium sulfate, after Fu Luoli silicon column solid phase extraction purifies, uses ECD after air inlet chromatography Detector detects, and carries out qualitative according to retention time, area quantified by external standard method.
As preferably, the present invention uses organophosphor, organochlorine and pyrethrin pesticide in gas chromatography determination rice sample The step of residual quantity is as follows:
1. extract
Edible rice dry sample, weighs the size-reduced rice sample of 5.0g, is placed in 250mL plastic centrifuge tube, adds 25.0mL distilled water, stands 30min, adds 25.0ml acetonitrile, is homogenized 2min, adds 10g anhydrous slufuric acid in high speed dispersor Magnesium and 1g sodium chloride, be homogenized 1 minute in low speed dispersion machine, and centrifugal force is 2500g, centrifugal 3min, makes acetonitrile and aqueous phase layering；
2. purify
Organophosphor purifies: pipettes 4.0ml upper strata acetonitrile solution and purifies in 15ml graduated centrifuge tube, to be measured；
Organochlorine and chrysanthemum ester purify: pipette 10ml upper strata acetonitrile solution in 15ml graduated centrifuge tube, in centrifuge tube in advance Adding 0.5g sodium chloride, vortex mixed 1min, stratification, accurately absorption 5ml acetonitrile solution is in boiling flask, and rotary evaporation is extremely Near dry, dissolve with the mixed liquor of the acetone+n-hexane of 2mL and obtain solution to be clean；
By Fu Luoli silicon post successively with the 5.0mL acetone+mixed liquor of n-hexane, the pre-drip washing of 5.0mL n-hexane, conditioning, When solvent liquid level arrives post adsorption layer surface, pour above-mentioned solution to be clean immediately into, receive eluting with 15mL graduated centrifuge tube Liquid, rinses drip washing Fu Luoli silicon post after beaker with the mixed liquor of 5mL acetone+n-hexane, and is repeated once；Leacheate will be filled Centrifuge tube is placed on Nitrogen evaporator, and under the conditions of bath temperature 50 DEG C, nitrogen blows and is evaporated to, less than 5mL, be settled to n-hexane 5.0mL, mixes on vortex mixer, to be measured；
During for using automatic solid-phase extractor to purify, take the above-mentioned supernatant 8mL saltoutd, at rotary evaporation extremely After the most dry, the mixed liquor adding acetone+n-hexane dissolves and is settled to 8mL, and instrument loading 2.5mL, with 4mL acetone+n-hexane Mixed liquor drip washing Fu Luoli silicon post at twice, the centrifuge tube filling leacheate is placed on Nitrogen evaporator, bath temperature 50 DEG C Under the conditions of, nitrogen blows and is evaporated to, less than 2mL, be settled to 2.5mL with n-hexane, mixes on vortex mixer, to be measured；
In the mixed liquor of acetone+n-hexane, the volume ratio of acetone and n-hexane is 1:9；
3. organophosphor measures
Chromatographic condition is as follows:
Chromatographic column: DB-1701 quartz capillary column, 30m × 0.25mm × 0.25um；
Column temperature: initial temperature 90 DEG C, rises to 270 DEG C with 25 DEG C/min immediately, keeps 3min；
Injection port: temperature 250 DEG C, pressure 25psi；
Sample size: 1ul；
Input mode: pulse does not shunts, pulsating pressure 50psi, keep 1min, purge time 0.9min；
Detector temperature: 240 DEG C；
Gas: carrier gas N2, constant voltage 25psi；H2Flow velocity 120ml/min；Air velocity 88ml/min；
Sample determination
Chromatographic condition in pressing 3. is to standard working solution and sample solution equal-volume sample introduction, qualitative according to retention time, face Long-pending quantified by external standard method；
4. organochlorine and chrysanthemum ester measure
Chromatographic condition is as follows:
Chromatographic column: DB-17 or DB-1 quartz capillary column, 30m × 0.25mm × 0.25um；
Column temperature: initial temperature 90 DEG C, rises to 150 DEG C with 25 DEG C/min immediately, then rises to 270 DEG C with 10 DEG C/min, keeps 8min；
Injection port: temperature 250 DEG C, pressure 30psi；
Sample size: 1ul；
Input mode: shunting, split ratio is 5:1；
Detector temperature: 300 DEG C, post flow+tail wind drift amount=30mL/min；
Gas: carrier gas N2, constant voltage 30psi；
5. sample determination
Chromatographic condition in pressing 4. is to standard working solution and sample solution equal-volume sample introduction, qualitative according to retention time, face Long-pending quantified by external standard method；
6. result calculates
In rice sample, tested pesticide concentration is in terms of mass fraction W, and numerical value is milligrams per kilogram to represent, based on following equation Calculate:
W = A 1 × C × V 2 × V A × V 1 × V 4 V 3 × m
V1-standard specimen sampling volume, μ l；
V2-sample feeding volume, μ l；
A-standard specimen peak area；
A1-sample peak area；
M-sample quality (g)；
V3-solvent adds volume (ml)；
V4-point take solvent volume (ml)；
V-constant volume (ml).
As preferably, in step of the present invention (2), use organophosphor in liquid chromatograph/concatenation mass spectrometric determination rice sample, Organic nitrogen, carbamate chemicals residual amount step as follows: rice sample Pesticides is through acetonitrile extraction, and extracting solution is through magnesium sulfate Saltout, after PSA dispersive solid-phase extraction purifies, with liquid chromatograph concatenation mass spectrograph detection, according to retention time and qualitative ion And quota ion and qualitative ion ratio carry out qualitative, quota ion area external standard method is carried out quantitatively.
As preferably, the present invention uses organophosphor, organic nitrogen, ammonia in liquid chromatograph/concatenation mass spectrometric determination rice sample The step of carbamate persticide residue is as follows:
1. extract
Edible rice dry sample, weighs the size-reduced rice sample of 5.0g, is placed in 250mL plastic centrifuge tube, adds 25.0mL distilled water, stands 30min；Add 25.0ml acetonitrile, high speed dispersor is homogenized 2min, adds 10g anhydrous slufuric acid Magnesium and 1g sodium chloride, be homogenized 1 minute in low speed dispersion machine, and centrifugal force is 2500g, centrifugal 3min, makes acetonitrile and aqueous phase layering；
2. purify
Pipette 4.0ml upper strata acetonitrile solution in 15ml graduated centrifuge tube, purify, to be measured；
3. instrument condition
Chromatographic condition is as follows:
Chromatographic column: ZORBAX SB C18 (100mm × 2.1mm, 1.8 μm)；
Column temperature: 55 DEG C；
Mobile phase A: the 5mmol/L ammonium acetate solution containing 0.1% formic acid；Mobile phase B: acetonitrile；
Flow velocity: 0.3mL/min；
Mass Spectrometry Conditions is as follows:
Ion source: ESI；
Capillary voltage: 4kV；
Nitrogen flow rate: 10L/min；
Mass spectrum acquisition rate: 500ms/cycle；
Nebulizer pressure: 35psi；
Dry temperature: 350 DEG C；
4. sample determination
By the instrument condition in 3. to standard working solution and sample solution equal-volume sample introduction, according to retention time and qualitative from Son and quota ion and qualitative ion ratio carry out qualitative, and quota ion area external standard method is carried out quantitatively；
5. result calculates
In sample, tested pesticide concentration is in terms of mass fraction W, and numerical value, milligrams per kilogram to represent, is calculated by following equation:
W = A 1 × C × V 2 × V A × V 1 × V 4 V 3 × m
V1-standard specimen sampling volume, μ l；
V2-sample feeding volume, μ l；
A-standard specimen peak area；
A1-sample peak area；
M-sample quality (g)；
V3-solvent adds volume (ml)；
V4-point take solvent volume (ml)；
V-constant volume (ml).
As preferably, in step of the present invention (3), use the heavy metal cadmium in graphite oven atomic absorption detection edible rice The step of content is as follows:
1. prepared by sample
Removing the foreign material in rice sample, with quartering division to 50g after mixing, ground at least 98% passes through aperture The sieve of 0.180mm, standby after mixing；
2. Specimen eliminating
Weigh rice sample 0.5g to be placed in digester, add 5mL concentrated nitric acid, place 15min, build sealing lid, put into In microwave digestion system, rotate rotating disk 1min, clear up；After clearing up completely when screen instruction temperature is less than 50 DEG C, open The door of microwave dissolver, the most slowly unclamps explosion-proof membrane cover to discharge pressure, takes off temperature sensor, opens sealing lid, will disappear Solve liquid transfer constant volume in 25mL volumetric flask, mix to be measured；Do reagent blank simultaneously；
3. Specification Curve of Increasing
Utilize the automatic dilution function of graphite furnace automatic sampler, allow it automatically by the top mark aqueous standard method of cadmium element Curve, and add corresponding matrix modifier；Set the condition of instrument；Input relevant parameter, and design the dense of standard curve Degree gradient；Draw standard curve；
4. calculate
X=(c-c0) × V × 1000/m × 1000 × 1000
In formula: each constituent content, mg/kg in X-sample；
C treatments of the sample liquid measures concentration, ng/mL；
C0 sample blank Digestive system concentration, ng/mL；
V treatments of the sample liquid cumulative volume, mL；
M-sample quality, g.
As preferably, chalkiness degree, edible quality, persticide residue and heavy metal cadmium that the present invention obtains according to detection contain Amount, carries out quality grading to edible rice, specific as follows:
The present invention compared with prior art, has the following advantages and effect: 1, propose quality of rice safe class concept, for The agricultural industry criteria of system revision later provides scientific basis；2, be conducive to instructing the production of China's rice product, consumption.Producer Can fix a price by credit rating, consumer can be chosen purchase, can really embody high quality and favourable price.3, High Quality Environment could produce excellent Matter rice, has had quality grading, and High Quality Environment is worth and emerges from, and is conducive to preserving the ecological environment and the sustainable development of agricultural Exhibition.4, the detection method of persticide residue and heavy metal cadmium content has that speed is fast, accuracy is high, and reagent saves, environmentally friendly, Also have stability and reproducible feature.
Accompanying drawing explanation
Fig. 1 is chalkiness degree testing result image local schematic diagram in the embodiment of the present invention.
Fig. 2 is the preparation process schematic diagram of cadmium standard solution and standard curve in the embodiment of the present invention.
Detailed description of the invention
The present invention is described in further detail below in conjunction with the accompanying drawings and by embodiment, and following example are to this Bright explanation and the invention is not limited in following example.
Embodiment.
The present embodiment needs to select pesticide residues, heavy metal cadmium, edible product around safety, nice, good-looking substantive markets Matter, chalkiness degree are as value parameter, and its stage division is as follows:
Edible Semen Oryzae quality grading method
One, value parameter explanation
Quality of rice is a comprehensive concept, substantially sub-argumentization and safely two classes in index: physical and chemical index divides mills Quality, exterior quality, cooking and eating quality and nutritional quality.Milled quality mainly includes brown rice yield (also known as Coarse Rice Rate), polished rice Rate and head rice rate, the processing characteristics of dominant response rice；Exterior quality mainly includes shape, size, transparency and chalkiness degree, The appearance characteristics of dominant response rice；Cooking and eating quality includes the gelatinization point of rice, gel consistence, amylose content, food Flavor quality, the cooking property of dominant response rice and food flavor sense organ；Nutritional quality includes protein, fat, vitamin, mineral Deng, the nutrition of reaction rice.
In above-mentioned physical and chemical quality index, can represent good-looking index is chalkiness degree.
Chalkiness degree: for one of the most important index of Appearance Quality of Paddy Rice, wherein, chalk is White-opalescent in rice endosperm in vain Part, in order there is space between endosperm starch grain, to cause light transmission to change caused.The position occurred on seed in vain according to chalk Difference, is generally divided into that white belly, the back of the body be white and the type such as core white, domestic use chalkness ratio, Chalkiness size, three conceptual descriptions of chalkiness degree The white situation of chalk.Chalkiness degree is the percentage ratio that in rice, the area at the white position of chalk accounts for grain of rice projected area.Chalkiness degree not only closes in fact It is tied to the whether goodlooking of rice, processing quality, cooking quality are also had a significant impact.
Can represent nice index edible quality.
Edible quality: rice edible quality be rice during processed and edible time shown color and luster, abnormal smells from the patient, taste The concentrated expression of the characteristics such as taste, rice viscosity and soft or hard palatability.It it is the most important index of quality of rice.Its paste with rice Change the physical and chemical index such as temperature, gel consistence, amylose content to be correlated with, be also rice variety, plantation level, processing technique, the oldest The concentrated expression of the influencing factors of quality such as degree.
Safety index is mainly pesticide residues and heavy metal:
Pesticide residues: pesticide residues are problems the most complicated, and on Oryza sativa L., common pesticides reaches hundreds of, and uses every year Pesticide all in change, novel pesticide continues to bring out, and is difficult to be used as value parameter with certain concrete pesticide, but according to whole nation rice Meter Zhi Liang generaI investigation and risk assessment monitoring result are seen, China's rice residual recall rate of product agriculture is up to more than 20%, and many products are examined Go out Multiple Pesticides, pesticide detection number reflect production process Pesticides use, the practical situation of safety interval control etc., Therefore, using pesticide detection number as graded index simple possible.The year that the pesticide parameter of concrete detection can be issued according to the Ministry of Agriculture Degree quality of rice security risk assessment detection parameter depending on, as 2015 detection 52 kinds of pesticide be: Bayer 71628, parathion-methyl, Isofenphos methyl, Azodrin, quintiofos, Rogor, phosphamidon, Malathion, phonamiphos, triazophos, fenifrothion, isocarbophos, Phosmet, orthene, Bravo, clofenotane, Gamma Hexaochlorocyclohexane, triazolone, Buprofezin, tricyclazole, Triadimenol, phoxim, Acetochlor, isopropyl methoxalamine, Mobucin, butachlor, chlorpyrifos-methyl, phenthoate dimephenthoate cidial, dichlorvos, chlopyrifos, parathion, diazine Phosphorus, decis, cypermethrin, iprobenfos, Ethodan, Difenoconazole, imidacloprid, Isoprothiolane, metrifonate, Acetamiprid, Avilamycin, carbendazim, paclobutrazol, ethiprole, alachlor, thiophanate-methyl, carbaryl, metalaxyl, carbofuran, Prochloraz, Diacloden.
Heavy metal: on Oryza sativa L., the heavy metal of generally detection has cadmium, lead, arsenic, hydrargyrum, chromium etc., and wherein cadmium is recall rate, exceeding standard rate The highest, the statistical result of 2003-2012 whole nation quality of rice Survey Sample is being shown, the recall rate of cadmium reaches 97%, rice In meter, the height of cadmium content substantially reflects the pollution situation in water and soil compression ring border, rice district, place, therefore, it can the height of cadmium content Low as graded index.The highest limitation of cadmium during 0.2mg/kg is GB rice in graded index is that Cd concentration of brown rice is up to standard to be wanted Ask；0.1mg/kg is the average of Survey Sample cadmium, and as the starting point of premium grade, sample compliance rate is 65%；0.01mg/kg's Sample compliance rate is 16%；The sample compliance rate of 0.05mg/kg is 48%.
Two, the detection of value parameter
(1) mensuration of rice whiteness measuring
1, principle:
Use picture imaging techniques and the automatic cutting techniques of elongated target, identify that chalk is white in conjunction with artificial guiding, measure rice Chalkiness degree.
2, instrument and equipment
Test luxurious paddy machine, experiment rice mill, riffle sampler, electronic balance (sensibility reciprocal 0.01g), bolter of cracking rice, image scanning Instrument, band Rice Outer-quality analyze the computer of software.
3, prepared by sample
Paddy husking becoming brown rice, then is milled into the polished rice that precision is national standard three grades, with cracking rice, bolter separates broken Rice, separates the sample after cracking rice and sorts the most further and stay length to reach sample complete grain of rice average length 3/4ths The grain of rice i.e. head milled rice more than and is standby.
4, the mensuration of chalkiness degree
Dividing with riffle sampler and take 10g～35g sample, be placed in by sample on scanner glass plate, weak vibrations causes between the grain of rice Scatter and the most overlapping, scanned sample, it is thus achieved that rice Sample Image, from scanning figure automated randomized choose complete no less than 100 Polished rice Sample Image, is aided with artificial rejecting and stays skin or embryo to be judged to the grain of rice image that chalk is white, finally by rice outward appearance product on sample by mistake Matter is analyzed computed in software and is gone out chalkiness degree, and scanogram sees Fig. 1.Replication Duplicate Samples.
5, result represents
Result of calculation represents with the arithmetic mean of instantaneous value of parallel assay, retains 1 decimal.
6, allowable error
Chalkiness degree parallel assay difference≤1.5%.
(2) mensuration of rice edible quality
Sensory evaluation method measures rice edible quality.Rice sample after steaming and decocting becomes rice under prescribed conditions, judges personnel By observing, nose is heard, mouth tastes etc. that color and luster, the gas of surveyed rice are hidden by method, flavour, rice viscosity and soft or hard palatability are carried out The comprehensive process tasting evaluation.
1, principle
Oryza glutinosa, through rice huller paddy, pearling, is prepared as the rice of national standard three equally accurate as sample.Commodity rice directly as Sample.Taking a certain amount of sample, steaming and decocting becomes rice under prescribed conditions, and the abnormal smells from the patient of the sensory test rice of the personnel that judge, outward appearance are tied Structure, palatability, flavour and cold meal quality etc., evaluation result represents with the meansigma methods participating in the comprehensive grading judging personnel.
2, key instrument and utensil
2.1 steamed rice ware: more than 60mL aluminum with cover (or rustless steel) box.
2.2 directly-heated type electric cookers: 3L, 500W.
3, operating procedure
Prepared by 3.1 samples
Oryza glutinosa sample is prepared as the rice of three equally accurate.Commodity rice the most directly divides materialses.
The numbering of 3.2 samples and registration
The numbering of random layout sample, prepare rice box number or pot number.
The preparation of 3.3 rice
3.3.1 the preparation of low-volume samples rice
3.3.1.1 sample is claimed: weigh every part of 10g sample in dewatering screen.Sample number is prepared by everyone l part of valuation officer.
3.3.1.2 wash rice: be placed in basin by dewatering screen, rapidly join 150mL tap water, the most clockwise stirring 10 circle, Stirring 10 circle counterclockwise, quick water change repeats aforesaid operations once.Again with 150mL aquae destillata drip washing 1 time, the most remaining water of drip, people In the steamed rice ware of corresponding numbering.Washing meter time controls at 3min-5min.
3.3.1.3 soak: Semen Oryzae adds 1.6 times that the distilled water yield is sample size, and Semen oryzae sativae adds 1.3 that the distilled water yield is sample size Times.Amount of water suitably can increase and decrease according to rice soft or hard.Soak water temperature about 25 DEG C, soak time 30min.
3.3.1.4 steaming and decocting: add appropriate water in steamer, be heated to boiling with electric furnace ＜ or electromagnetic oven ＞, take off pot cover, then The steamed rice ware holding sample is added a cover on placement steaming tray, cover pot cover, continue heating and start timing, steaming and decocting 40min, stopping adding Heat, vexed meal 20min.
3.3.2 the preparation of a large amount of sample rice
3.3.2.1 sample is claimed: weigh every part of 500g.
3.3.2.2 rice is washed: the 500g sample weighed is put into dewatering screen, is placed in basin by dewatering screen, rapidly joins 1500ml tap water, the most clockwise stirring 10 circle, counterclockwise stirring 10 circle, quick water change repeats aforesaid operations once.Use again 1500mL aquae destillata drip washing 1 time, the most remaining water of drip, in the directly-heated type electric cooker that people numbers accordingly.Washing meter time controls at 3- 5min。
3.3.2.3 steaming and decocting: electric cooker switches on power beginning cooking rice, must not open pot cover in digestion process.Electricity meal After the switch tripping of pot, more vexed 20min processed.
3.3.2.4 rice is stirred: spoon of having a meal stirs well-done rice, first loosens from the periphery of pot, makes rice and pot wall Separate, then by each parallel sliding of both direction 2 times anyhow, then stir up and down with chopsticks 4 times, after making unnecessary moisture evaporation Cover pot cover, more vexed 10min.
3.3.2.5 about 50g sample rice is loosely contained in little bowl, everyone 1 part, then tip upside down on white porcelain service plate Different positions, in bacterium taper, judges while hot.
3.4 samples are judged
3.4.1 content is judged: judge the abnormal smells from the patient of rice, surface structure, palatability (including viscosity, elasticity, soft durometer), grow Taste and cold meal quality.
3.4.2 personnel are judged: being made up of 5-10 preferred valuation officers, each valuation officer is numbered with number, is divided into some groups. Valuation officer before judging non-smoking in 1h, live on air, but can drink water；During judging, there is normal physiological status, do not make Apply some make up or other have the articles for use of obvious abnormal smells from the patient.
3.4.3 order and requirement are judged
3.4.3.1 the preparation before judging: valuation officer gargles by warm water before judging every time, gargles the residue in mouth.
3.4.3.2 distinguish that rice gas is hidden: be placed in below nasal cavity by rice while hot, the most at full tilt air-breathing, carefully distinguish rice The abnormal smells from the patient of meal.
3.4.3.3 rice outward appearance is observed: observe the color on rice surface, gloss and rice grain integrity.
3.4.3.4 distinguish the palatability of rice: take rice with chopsticks and put into a little in mouth, chew carefully, chew while with tooth, tongue First-class each sensory organ carefully tastes the items such as the viscosity of rice, soft durometer, elasticity, flavour.
The coldest meal quality: after rice at room temperature places 1h, tastes and judges the viscoelasticity of cold meal, bonding conglobation property And hardness.
3.5 scoring
3.5.1 methods of marking
3.5.1.1 hide according to the gas of rice, surface structure, palatability, flavour and cold meal quality, mark, comprehensively comment It is divided into every score sum.Code of points and log form see table.
Rice sensory evaluation code of points and record
Judge group #: name: sex: the age:
Judge the time: the date time-division
3.5.1.2 calculating meansigma methods according to the comprehensive grading result of each valuation officer, indivedual valuation officers judge the big person of error (exceeding average more than 10 points) can be given up, and recalculates meansigma methods after giving up.Finally using the meansigma methods of comprehensive grading as rice The result of edible quality subjective appreciation, result of calculation round numbers.Following table is result statistical table.
4 judge
Comprehensive grading is with more than 90 points for excellent (one-level), and 81 point-90 is divided into (two grades), and 71 point-80 is divided into preferably (three Level), 61 point-70 is divided into general (level Four), and 51 point-60 is divided into poor (waiting outer).
(3) mensuration of organophosphor, organochlorine and Determining pyrethroid pesticide residues in rice: gas chromatography.
1 method summary
In sample, organophosphor, organochlorine and pyrethrin pesticide are saltoutd through magnesium sulfate through acetonitrile extraction, extracting solution, divide through PSA After dissipating Solid phase extraction, detect with FPD detector after air inlet chromatography, carry out qualitative according to retention time, area external standard Standard measure.
In sample, organochlorine and pyrethrin pesticide are saltoutd through magnesium sulfate through acetonitrile extraction, extracting solution, solid through Fu Luoli silicon post After phase extracting and purifying, detecting with ECD detector, carry out qualitative according to retention time after air inlet chromatography, area external standard is legal Amount.
2 measurement ranges
Organophosphorus insecticide includes: dichlorvos, Bayer 71628, orthene, thimet, omethoate, Azodrin, pleasure Really, chlopyrifos, parathion-methyl, Malathion, fenifrothion, parathion, quintiofos, isocarbophos, triazophos, fenthion, Diazinon, cadusafos, methidathion, phosmet, Isofenphos methyl etc..
Organochlorine and pyrethrin pesticide include: Gamma Hexaochlorocyclohexane, clofenotane, cypermethrin, fenvalerate, Fenpropathrin, chlorine chrysanthemum Ester, lambda-cyhalothrin, cyfloxylate, decis, Biphenthrin, taufluvalinate, flucythrinate, triazolone, hundred bacterium Clearly, RP-26019, dicofol, procymidone, pentachloronitrobenzene, vinclozolin etc..
3 reagent
3.1 acetonitriles: the residual level of agriculture, the U.S. world (TEAIA).
3.2 acetone: the residual level of agriculture, the U.S. world (TEAIA).
3.3 normal hexane: the residual level of agriculture, the U.S. world (TEAIA).
3.4 toluene: the residual level of agriculture, the U.S. world (TEAIA).
3.5 magnesium sulfate: two kinds of magnesium sulfate are used in this experiment, and one is purity ＞ 97%, graininess (20～50 mesh), lark Prestige ACROS product, because it has graininess, will not cause dust in experimentation, be mainly used in saltouing.Another kind of residual for agriculture Level, powder (100 mesh), U.S.'s Alfa Products, because of its powder, soaking effect is good, for dehydration (because of its be Sealed tube is carried out, it is not necessary to consider dust problem).
3.6 sodium chloride: the residual level of agriculture, Germany's CNW product.
3.7 γ-gulonolactone.
3.8 protective agent solution: weigh γ-gulonolactone 100mg in 10ml volumetric flask, add 2ml water and are allowed to molten Solve, be then settled to 10ml with acetonitrile, mixing, cross the 0.22 organic filter membrane of μm, standby.
3.9 standard sample of pesticide: country's certified reference material (usual concentration is 1000 or 100mg/L)；Import sterling standard specimen (the high concentration list mark storing solution of 1000mg/L need to be configured to).
3.10 standard working solution: organophosphorus pesticide standard mixed solution acetontrile becomes the standard of 0.25mg/L to work Solution, is placed in-20 DEG C of preservations.Before measuring, standard specimen is added by standard working solution+protective agent mixed liquor (10:1 mixing by volume) Enter protective agent mixed solution, mixing.
Organochlorine and chrysanthemum ester standard mixed solution normal hexane are configured to the standard working solution of 0.1mg/L, are placed in-20 DEG C Preserve.
4 instruments
4.1 gas chromatograpies (attached FPD and ECD detector).
4.2 high speed dispersor.
4.3 centrifuge.
4.4 balance.
4.5 turbine mixer.
5 analytical procedures
5.1 extract
Rice Samples dry sample, weighs the size-reduced sample of 5.0g, is placed in 250mL plastic centrifuge tube, adds 25.0mL and steams Distilled water, stands 30min.Add 25.0ml acetonitrile, high speed dispersor high speed be homogenized 2min, add 10g anhydrous magnesium sulfate and 1g sodium chloride, in low speed dispersion machine, low speed is homogenized 1 minute (substituting shaking step), and centrifugal force is that 2500g is centrifuged 3min, makes second Nitrile and aqueous phase layering.
5.2 purify
5.2.1 organophosphor
Pipette 4.0ml upper strata acetonitrile solution in 15ml graduated centrifuge tube, centrifuge tube adds 100mgPSA and C-in advance 18,1200mg anhydrous magnesium sulfate, after vortex mixed 1min, 3000 revs/min of centrifugal 5min.Accurately draw 0.8ml acetonitrile solution In sample injection bottle, and add protective agent solution 0.08ml, shake up, to be measured.
5.2.2 organochlorine and chrysanthemum ester
Pipette 10ml upper strata acetonitrile solution in 15ml graduated centrifuge tube, centrifuge tube adds 0.5g sodium chloride, whirlpool in advance Rotation mixing 1min, stratification.Accurately draw 5ml acetonitrile solution, to use to nearly dry (about 0.3mL) in boiling flask, rotary evaporation The mixed liquor (volume ratio of acetone and n-hexane is 10:90) of the acetone+n-hexane of about 2mL dissolves, to be clean.
By Fu Luoli silicon post successively with the mixed liquor of 5.0mL acetone+n-hexane (volume ratio of acetone and n-hexane is 10: 90), the pre-drip washing of 5.0mL n-hexane, conditioning, when solvent liquid level arrive post adsorption layer surface time, pour into above-mentioned to be clean immediately Solution, receives eluent with 15mL graduated centrifuge tube, by mixed liquor (acetone and the volume ratio of n-hexane of 5mL acetone+n-hexane For 10:90) rinse drip washing Fu Luoli silicon post after beaker, and be repeated once.The centrifuge tube filling leacheate is placed on Nitrogen evaporator, Under the conditions of bath temperature 50 DEG C, nitrogen blows and is evaporated to, less than 5mL, be settled to 5.0mL with n-hexane, mixed on vortex mixer Even, to be measured.
During for using automatic solid-phase extractor to purify, take the above-mentioned supernatant 8mL saltoutd, at rotary evaporation extremely Nearly dry rear (about 0.5mL), the mixed liquor (volume ratio of acetone and n-hexane is 10:90) of the acetone+n-hexane adding 7.5mL is molten Solving (constant volume is 8mL), instrument loading 2.5mL, by mixed liquor (acetone and the volume ratio of n-hexane of 4mL acetone+n-hexane For 10:90) drip washing Fu Luoli silicon post at twice, the centrifuge tube filling leacheate is placed on Nitrogen evaporator, bath temperature 50 DEG C Under the conditions of, nitrogen blows and is evaporated to, less than 2mL, be settled to 2.5mL with n-hexane, mixes on vortex mixer, to be measured.(keep dilute Release multiple constant)
5.3 organophosphors measure
5.3.1 chromatographic condition
5.3.1.1 chromatographic column: DB-1701 quartz capillary column, 30m × 0.25mm × 0.25um.
5.3.1.2 column temperature: initial temperature 90 DEG C, rises to 270 DEG C with 25 DEG C/min immediately, keeps 3min.
5.3.1.3 injection port: temperature 250 DEG C, pressure 25psi.
5.3.1.4 sample size: 1ul.
5.3.1.5 input mode: pulse does not shunts, pulsating pressure 50psi, keep 1min, purge time 0.9min.
5.3.1.6 detector temperature: 240 DEG C.
5.3.1.7 gas: carrier gas N2, constant voltage 25psi；H2Flow velocity 120ml/min；Air velocity 88ml/min.
5.3.2 sample determination
By 5.3 instrument conditions, to standard working solution and sample solution equal-volume sample introduction, qualitative according to retention time, area Quantified by external standard method.
5.4 organochlorine and chrysanthemum ester measure
5.4.1 chromatographic condition
5.4.1.1 chromatographic column: DB-17 or DB-1 quartz capillary column, 30m × 0.25mm × 0.25um.
5.4.1.2 column temperature: initial temperature 90 DEG C, rises to 150 DEG C with 25 DEG C/min immediately, then rises to 270 DEG C with 10 DEG C/min, protects Hold 8min.
5.4.1.3 injection port: temperature 250 DEG C, pressure 30psi.
5.4.1.4 sample size: 1ul.
5.4.1.5 input mode: shunting, split ratio is 5:1.
5.4.1.6 detector temperature: 300 DEG C, post flow+tail wind drift amount=30mL/min.
5.4.1.7 gas: carrier gas N2, constant voltage 30psi.
5.4.2 sample determination
By 5.4 instrument conditions, to standard working solution and sample solution equal-volume sample introduction, qualitative according to retention time, area Quantified by external standard method.
6 results calculate
In sample, tested pesticide concentration is in terms of mass fraction W, and numerical value represents with milligrams per kilogram (mg/kg), by following public affairs Formula calculates:
W = A 1 × C × V 2 × V A × V 1 × V 4 V 3 × m
V1-standard specimen sampling volume, μ l.
V2-sample feeding volume, μ l.
A-standard specimen peak area.
A1-sample peak area.
M-sample quality (g).
V3-solvent adds volume (ml).
V4-point take solvent volume (ml).
V-constant volume (ml).
Result of calculation retains two position effective digitals, retains three position effective digitals when result is more than 1mg/kg.Measured value The revision of the convention of computing and Effective Numerical is carried out by numerical value rule for rounding off.
(4) in rice, the persticide residue such as organophosphor, organic nitrogen, carbamate measures: liquid chromatograph/concatenation mass spectrum Method.
1 method summary
Rice sample Pesticides is saltoutd through magnesium sulfate through acetonitrile extraction, extracting solution, after PSA dispersive solid-phase extraction purifies, With phase chromatography-use concatenation mass spectrograph detection, carry out according to retention time and qualitative ion and quota ion and qualitative ion ratio Qualitative, quota ion area external standard method is carried out quantitatively.
2 measurement ranges
80 kinds of pesticide include: 3-hydroxyl carbofuran, avilamycin, orthene, Acetamiprid, Acetochlor, alachlor, tears Go out prestige, Aldicarb sulfone, Tinidazole glucose injection, atrazine, Fluoxastrobin, Buprofezin, butachlor, carbaryl, carbendazim, carbofuran, fluorine Pyridine urea, d ichlorbenzuron, chlopyrifos, chlorpyrifos-methyl, cyflufenamid, diazinon, dichlorvos, Difenoconazole, diflubenzuron, Rogor, Dimethomorph, Ethodan, fenamiphos, fenifrothion, fenthion, ethiprole, Cascade, bis(4-fluorophenyl)methyl(1H-1,2,4-triazol-1-ylmethyl)silane, HEXAFLUMURON, Hexythiazox, press down Mould azoles, imidacloprid, indoxacarb, RP-26019, isocarbophos, Mobucin, Isoprothiolane, lufenuron, Malathion, metalaxyl, methylamine Phosphorus, methidathion, Methomyl, methoxyfenozide, isopropyl methoxalamine, Azodrin, omethoate, paclobutrazol, parathion, methyl are to sulfur Phosphorus, Pendimethalin, thimet, Phosalone, phosmet, phoxim, Aphox, Prochloraz, propargite, N-phenyl isopropyl carbamate, third Ring azoles, pyridaben, pyrimethanil, quintiofos, Quizalotop-ethyl, multiple killing teichomycin-A, multiple killing teichomycin-B, tebufenozide, probenazole, thiophene worm Piperazine, thiophanate-methyl, triazolone, Triadimenol, triazophos, metrifonate, tricyclazole.
3 reagent
3.1 acetonitriles: the residual level of agriculture, the U.S. world (TEAIA).
3.2 acetonitriles: liquid chromatographic grade, MERCK.
3.3 magnesium sulfate: two kinds of magnesium sulfate are used in this experiment, and one is purity ＞ 97%, graininess (20～50 mesh), lark Prestige ACROS product, because it has graininess, will not cause dust in experimentation, be mainly used in saltouing.Another kind of residual for agriculture Level, powder (100 mesh), U.S.'s Alfa Products, because of its powder, soaking effect is good, for dehydration (because of its be Sealed tube is carried out, it is not necessary to consider dust problem).
3.4 sodium chloride: analytical pure, Germany's CNW product.
3.5 PSA: U.S.'s Varian.
3.6 C-18: U.S.'s Varian.
3.7 ammonium acetates: U.S. Sigam-FLUKA.
3.8 formic acid: the chromatographically pure U.S. world (TEAIA).
3.9 standard sample of pesticide: country's certified reference material (usual concentration is 1000 or 100mg/L)；Import sterling standard specimen (the high concentration list mark storing solution of 1000mg/L need to be configured to).
3.10 standard mixed solution acetontrile become the standard working solution of 0.1mg/L, are placed in-20 DEG C of preservations.
4 instruments
4.1 Agilent6410B LC/MS/MS。
4.2 high speed dispersor.
4.3 centrifuge.
4.4 balance.
4.5 turbine mixer.
5 analytical procedures
5.1 extract
Rice Samples dry sample, weighs the size-reduced sample of 5.0g, is placed in 250mL plastic centrifuge tube, adds 25.0mL and steams Distilled water, stands 30min.Add 25.0ml acetonitrile, high speed dispersor high speed be homogenized 2min, add 10g anhydrous magnesium sulfate and 1g sodium chloride, in low speed dispersion machine, low speed is homogenized 1 minute (substituting shaking step), and centrifugal force is that 2500g is centrifuged 3min, makes second Nitrile and aqueous phase layering.
5.2 purify
Pipette 4.0ml upper strata acetonitrile solution in 15ml graduated centrifuge tube, centrifuge tube adds 100mgPSA and C-in advance 18,1200mg anhydrous magnesium sulfate, after vortex mixed 1min, 3000 revs/min of centrifugal 5min.Through 0.22 μm filtering with microporous membrane, To be measured.
5.3 instrument condition
5.3.1 chromatographic condition:
5.3.1.1 chromatographic column: ZORBAX SB C18 (100mm × 2.1mm, 1.8 μm)；
5.3.1.2 column temperature: 55 DEG C；
5.3.1.3 mobile phase A: the 5mmol/L ammonium acetate solution containing 0.1% formic acid；Mobile phase B: acetonitrile；
5.3.1.4 gradient elution program:
Time (min) Solvent orange 2 A (%) Solvent B (%)
0 80 20
13 10 90
15 10 90
15.1 80 20
21 80 20
5.3.1.5 flow velocity: 0.3mL/min；
5.3.1.6 sample size: auto-programming sample introduction (1 μ L sample liquid+4 μ L mobile phase A mixing, wash sample introduction after pin)；
5.3.2 Mass Spectrometry Conditions:
5.3.2.1 ion source: ESI；
5.3.2.2 capillary voltage: 4kV；
5.3.2.3 nitrogen flow rate: 10L/min；
5.3.2.4 mass spectrum acquisition mode: dynamically multiple-reaction monitoring (Dynamic MRM)；
5.3.2.5 mass spectrum acquisition rate: 500ms/cycle；
5.3.2.6 nebulizer pressure: 35psi；
5.3.2.7 be dried temperature: 350 DEG C.
5.3.2.8 mass spectrum acquisition parameter
5.4 sample determination
By 5.3 instrument conditions, to standard working solution and sample solution equal-volume sample introduction, according to retention time and qualitative ion And quota ion and qualitative ion ratio carry out qualitative, quota ion area external standard method is carried out quantitatively.
6 results calculate
In sample, tested pesticide concentration is in terms of mass fraction W, and numerical value represents with milligrams per kilogram (mg/kg), by following public affairs Formula calculates:
W = A 1 × C × V 2 × V A × V 1 × V 4 V 3 × m
V1-standard specimen sampling volume, μ l.
V2-sample feeding volume, μ l.
A-standard specimen peak area.
A1-sample peak area.
M-sample quality (g).
V3-solvent adds volume (ml).
V4-point take solvent volume (ml)
V-constant volume (ml).
Result of calculation retains two position effective digitals, retains three position effective digitals when result is more than 1mg/kg.Measured value The revision of the convention of computing and Effective Numerical is carried out by numerical value rule for rounding off.
(5) Cadmium detrmination in rice: graphite oven atomic absorption
1 method summary
Sample is after acid is cleared up, in graphite furnace automatic sampler imports atomic absorption spectrophotometer graphite furnace, through stone After ink stove high temperature atomic, Atomic Absorption specific wavelength spectral line in the optical path, its absorbance is directly proportional to its content.
2 instrument and equipments
2.1 U.S. CE M company MARS5 microwave dissolver.
2.2 power & light company of U.S. Sollar M6 Atomic Absorption Spectrometers (band FS95 graphite furnace automatic sampler).
2.3 cadmiums, lead, chromium, nickel hollow cathode lamp.
2.4 small-sized electric bruishers.
2.5 steel cylinder nitrogen (99.999%) or argon (99.999%).
2.6 circulating water devices (temperature is 15 DEG C).
2.7 volumetric flask, 25mL.
2.8 balances, sensibility reciprocal is 0.001g.
3 reagent
In this method, in addition to particular provisions, agents useful for same is that top grade is pure, and test water is high purity water.
3.1 nitric acid (technique is ultrapure).
3.2 perchloric acid.
3.3 nitric acid (1+99) (technique is ultrapure): measure 1.0mL nitric acid (4.1), add in 100mL volumetric flask, fixed with water Hold.
3.4 palladium nitrate solutions (0.5g/L): weigh 0.05g Palladous nitrate., with nitric acid (4.3) dissolved dilution to 100mL.
3.5 magnesium nitrate solutions (10g/L): weigh 1.0g magnesium nitrate, be diluted to 100mL with water dissolution.
3.6 ammonium sulfate (20g/L): weigh 2.0g ammonium sulfate, be diluted to 100mL with water dissolution.
3.7 cadmium Standard Reserving Solution: State Environmental Protection Administration's standard sample institute produces, and concentration is 100mg/L.Open Store in afterwards in refrigerator, preserve 1 year.
Cadmium standard solution and the compound method of standard curve and preservation are as shown in Figure 2.
4 operating procedures
Prepared by 4.1 samples
Removing foreign material in sample, with quartering division to about 50g after mixing, ground at least 98% passes through aperture 0.180mm (80 mesh) nylon mesh, stores in polyethylene bottle or polyethylene plastic bag after mixing, standby.
4.2 Specimen eliminating microwave digestion methods
Weigh rice sample 0.5g, be placed in digester, add 5mL concentrated nitric acid, place 15min, build sealing lid, put into In microwave digestion system, rotate rotating disk about 1min, check whether pressure transducer kinks.The program arranged according to table 1 is cleared up.Disappear After changing completely when screen instruction temperature is less than 50 DEG C, open the door of microwave dissolver, the most slowly unclamp explosion-proof membrane cover to release Bleed off pressure power, take off temperature sensor, open sealing lid, by digestion solution transfer also constant volume to 25mL volumetric flask, mix to be measured.With Time do reagent blank.
Table 1 plant sample micro-wave digestion program
Project Power Temperature DEG C Pressure p si Pressure rising time min Retention time min
Parameter Automatically 180 350 15 10
Note: originally clearing up program based on temperature control, Stress control is auxiliary；The matrix Ying Ji of the batch sample simultaneously cleared up This is identical.
5 measure
5.1 Instrument measuring conditions are according to table 2
Table 2 Instrument measuring condition
The drafting of 5.2 standard curves
Utilize the automatic dilution function of graphite furnace automatic sampler (FS95), allow it automatically be joined by the top mark solution of cadmium element Standard curve processed, compound concentration is shown in Table 3, and adds corresponding matrix modifier.
The compound concentration of table 3 standard curve and the kind of matrix modifier and dosage
Element Cadmium
Top mark solution concentration (ug/L) 2.0
Standard 0.5
Curve 1.0
Concentration 1.5
(ug/L) 2.0
Matrix Palladous nitrate., 2.0uL
Modifier Ammonium sulfate, 2.0uL
5.3 instrument automatic result of calculation mode is measured
Set the optimum condition of instrument.Input following parameter: sample number into spectrum, sample quality, dilution volume, sample size, And design the Concentraton gradient of standard curve.After adjusting light path and regulating zero point, enter standard series and measure, draw standard bent Line.Before proceeding to sample determination, blank value measuring state can be entered back into, with sample blank Digestive system sample introduction, allow instrument take Its average is as the blank value at the button end.Subsequently can sequentially determining sample.Measure complete after, select " printed report " can will survey Determine result and carry out automatic printing.
6 calculate
X=(c-c0) × V × 1000/m × 1000 × 1000
In formula: each constituent content, mg/kg in X-sample；
C-treatments of the sample liquid measures concentration, ng/mL；
C0-sample blank Digestive system concentration, ng/mL；
V-treatments of the sample liquid cumulative volume, mL；
M-sample quality, g.
Result is stated: 1. the computing of measured value and the revision of the convention of Effective Numerical are carried out by numerical value rule for rounding off；2. significant figure The figure place of the significant figure that figure place is minimum with measuring instrument precision in method is identical, or reservation more than Limited Doses in sanitary standard one Position.
Above detection method has that speed is fast, accuracy is high, and reagent saves, environmentally friendly, also have stability and repeatability Good feature.
Three, grade judges
The lowest class index reached with Product checking index is for judging grade.I.e. testing result agriculture is residual, cadmium all reaches one Level be judged to one-level；If one of which is two grades, it is judged to two grades；The like.
Four, effect and meaning
1, propose quality of rice safe class concept, provide scientific basis for the agricultural industry criteria of system revision later.
2, be conducive to instructing the production of China's rice product, consumption.Producer can be fixed a price by credit rating, and consumer is optional Select purchase, can really embody high quality and favourable price.
3, High Quality Environment could produce high quality white rice, has had quality grading, and High Quality Environment is worth and emerges from, and is conducive to protecting Protect ecological environment and the sustainable development of agricultural.
Although the present invention is open as above with embodiment, but it is not limited to protection scope of the present invention, any ripe Know the technical staff of this technology, in the change made without departing from the spirit and scope of the invention and retouching, all should be belonged to this The protection domain of invention.

Claims (10)

1. an edible Semen Oryzae and the quality grading method of edible Semen oryzae sativae, it is characterised in that: the step of described method is as follows:
(1) rice sample is taken, the chalkiness degree of detection rice sample；
(2) rice sample is taken, the persticide residue in detection rice sample；
(3) rice sample is taken, the heavy metal cadmium content in detection rice sample；
(4) chalkiness degree, persticide residue and the heavy metal cadmium content obtained according to detection, carries out quality grading to rice.
Edible Semen Oryzae the most according to claim 1 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: described method Also comprise the steps: to take rice sample, the edible quality of detection rice sample；Then according to detecting chalkiness degree, the food obtained With quality, persticide residue and heavy metal cadmium content, rice is carried out quality grading.
Edible Semen Oryzae the most according to claim 1 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: step (1) In, the determination step of chalkiness degree is as follows: divides with riffle sampler and takes 10g～35g rice sample, rice sample is placed in scanner glass On plate, weak vibrations causes to scatter between the grain of rice and the most overlapping, scanned sample, it is thus achieved that rice Sample Image, from scanning figure automatically Randomly select no less than 100 complete polished rice Sample Images, be aided with and artificial reject that to stay skin or embryo to be judged to chalk rice sample white by mistake Grain of rice image, finally calculate chalkiness degree.
Edible Semen Oryzae the most according to claim 2 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: detection rice The step of the edible quality of sample is as follows:
Preparing of low-volume samples rice is as follows:
Claim sample: weigh every part of 10g sample in dewatering screen；
Washing rice: be placed in basin by dewatering screen, rapidly join 150mL tap water, stirring 10 circle, stirs 10 counterclockwise the most clockwise Circle, quick water change repeats aforesaid operations once；Again with 150mL aquae destillata drip washing 1 time, the most remaining water of drip, the steaming that people numbers accordingly In meal ware；Washing meter time controls at 3min-5min；
Soak: Semen Oryzae adds 1.6 times that the distilled water yield is sample size, and Semen oryzae sativae adds 1.3 times that the distilled water yield is sample size；Soak water temperature About 25 DEG C, soak time 30min；
Steaming and decocting: add appropriate water in steamer, be heated to boiling, take off pot cover, then the steamed rice ware holding sample is added a cover placement On steaming tray, cover pot cover, continue heating and start timing, steaming and decocting 40min, stop heating, vexed meal 20min, judge while hot；
Preparing of a large amount of sample rice is as follows:
Claim sample: weigh every part of 500g；
Wash rice: the 500g sample weighed is put into dewatering screen, is placed in basin by dewatering screen, rapidly join 1500ml tap water, Stirring 10 circle the most clockwise, counterclockwise stirring 10 circle, quick water change repeats aforesaid operations once；Drench with 1500mL aquae destillata again Washing 1 time, the most remaining water of drip, in the directly-heated type electric cooker that people numbers accordingly；Washing meter time controls at 3-5min；
Steaming and decocting: electric cooker switches on power beginning cooking rice, must not open pot cover in digestion process；The switch tripping of electric cooker After, more vexed 20min processed；
Stirring rice: spoon of having a meal stirs well-done rice, first loosens from the periphery of pot, makes rice separate with pot wall, then by horizontal stroke The perpendicular each parallel sliding of both direction 2 times, then stirs up and down with chopsticks 4 times, makes the pot cover of unnecessary moisture evaporation, then Vexed 10min；
50g sample rice is loosely contained in little bowl, everyone 1 part, then tips upside down on positions different on white porcelain service plate, in Bacterium taper, judges while hot.
Edible Semen Oryzae the most according to claim 1 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: step (2) In, use organophosphor, organochlorine and Determining pyrethroid pesticide residues, the inspection of persticide residue in gas chromatography determination rice sample Survey step is as follows: in rice sample, organophosphor, organochlorine and pyrethrin pesticide are saltoutd through magnesium sulfate through acetonitrile extraction, extracting solution, After PSA dispersive solid-phase extraction purifies, detect with FPD detector after air inlet chromatography, carry out qualitative according to retention time, face Long-pending quantified by external standard method；Or, in rice sample, organochlorine and pyrethrin pesticide are saltoutd through magnesium sulfate through acetonitrile extraction, extracting solution, After Fu Luoli silicon column solid phase extraction purifies, detecting with ECD detector after air inlet chromatography, it is fixed to carry out according to retention time Property, area quantified by external standard method.
Edible Semen Oryzae the most according to claim 1 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: use gas phase In chromatography determination rice sample, the step of organophosphor, organochlorine and Determining pyrethroid pesticide residues is as follows:
1. extract
Edible rice dry sample, weighs the size-reduced rice sample of 5.0g, is placed in 250mL plastic centrifuge tube, adds 25.0mL and steams Distilled water, stands 30min, adds 25.0ml acetonitrile, is homogenized 2min, adds 10g anhydrous magnesium sulfate and 1g chlorine in high speed dispersor Changing sodium, be homogenized 1 minute in low speed dispersion machine, centrifugal force is 2500g, centrifugal 3min, makes acetonitrile and aqueous phase layering；
2. purify
Organophosphor purifies: pipettes 4.0ml upper strata acetonitrile solution and purifies in 15ml graduated centrifuge tube, to be measured；
Organochlorine and chrysanthemum ester purify: pipette 10ml upper strata acetonitrile solution in 15ml graduated centrifuge tube, add in advance in centrifuge tube 0.5g sodium chloride, vortex mixed 1min, stratification, accurately absorption 5ml acetonitrile solution is in boiling flask, and rotary evaporation is to closely Dry, dissolve with the mixed liquor of the acetone+n-hexane of 2mL and obtain solution to be clean；
Fu Luoli silicon post is used the 5.0mL acetone+mixed liquor of n-hexane, the pre-drip washing of 5.0mL n-hexane successively, and conditioning, when molten When agent liquid level arrives post adsorption layer surface, pour above-mentioned solution to be clean immediately into, receive eluent with 15mL graduated centrifuge tube, use The mixed liquor of 5mL acetone+n-hexane rinses drip washing Fu Luoli silicon post after beaker, and is repeated once；The centrifugal of leacheate will be filled Pipe is placed on Nitrogen evaporator, and under the conditions of bath temperature 50 DEG C, nitrogen blows and is evaporated to, less than 5mL, be settled to 5.0mL with n-hexane, Mix on vortex mixer, to be measured；
During for using automatic solid-phase extractor to purify, take the above-mentioned supernatant 8mL saltoutd, at rotary evaporation near dry After, the mixed liquor adding acetone+n-hexane dissolves and is settled to 8mL, and instrument loading 2.5mL, with mixing of 4mL acetone+n-hexane Close liquid drip washing Fu Luoli silicon post at twice, the centrifuge tube filling leacheate is placed on Nitrogen evaporator, in 50 DEG C of conditions of bath temperature Under, nitrogen blows and is evaporated to, less than 2mL, be settled to 2.5mL with n-hexane, mixes on vortex mixer, to be measured；
In the mixed liquor of acetone+n-hexane, the volume ratio of acetone and n-hexane is 1:9；
3. organophosphor measures
Chromatographic condition is as follows:
Chromatographic column: DB-1701 quartz capillary column, 30m × 0.25mm × 0.25um；
Column temperature: initial temperature 90 DEG C, rises to 270 DEG C with 25 DEG C/min immediately, keeps 3min；
Injection port: temperature 250 DEG C, pressure 25psi；
Sample size: 1ul；
Input mode: pulse does not shunts, pulsating pressure 50psi, keep 1min, purge time 0.9min；
Detector temperature: 240 DEG C；
Gas: carrier gas N2, constant voltage 25psi；H2Flow velocity 120ml/min；Air velocity 88ml/min；
Sample determination
Chromatographic condition in pressing 3. is to standard working solution and sample solution equal-volume sample introduction, qualitative according to retention time, outside area Mark standard measure；
4. organochlorine and chrysanthemum ester measure
Chromatographic condition is as follows:
Chromatographic column: DB-17 or DB-1 quartz capillary column, 30m × 0.25mm × 0.25um；
Column temperature: initial temperature 90 DEG C, rises to 150 DEG C with 25 DEG C/min immediately, then rises to 270 DEG C with 10 DEG C/min, keeps 8min；
Injection port: temperature 250 DEG C, pressure 30psi；
Sample size: 1ul；
Input mode: shunting, split ratio is 5:1；
Detector temperature: 300 DEG C, post flow+tail wind drift amount=30mL/min；
Gas: carrier gas N2, constant voltage 30psi；
5. sample determination
Chromatographic condition in pressing 4. is to standard working solution and sample solution equal-volume sample introduction, qualitative according to retention time, outside area Mark standard measure；
6. result calculates
In rice sample, tested pesticide concentration is in terms of mass fraction W, and numerical value, milligrams per kilogram to represent, is calculated by following equation:
W = A 1 × C × V 2 × V A × V 1 × V 4 V 3 × m
V1-standard specimen sampling volume, μ l；
V2-sample feeding volume, μ l；
A-standard specimen peak area；
A1-sample peak area；
M-sample quality (g)；
V3-solvent adds volume (ml)；
V4-point take solvent volume (ml)；
V-constant volume (ml).
Edible Semen Oryzae the most according to claim 1 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: step (2) In, use organophosphor in liquid chromatograph/concatenation mass spectrometric determination rice sample, organic nitrogen, carbamate chemicals residual amount Step is as follows: rice sample Pesticides is saltoutd through magnesium sulfate through acetonitrile extraction, extracting solution, after PSA dispersive solid-phase extraction purifies, With liquid chromatograph concatenation mass spectrograph detection, it is fixed to carry out according to retention time and qualitative ion and quota ion and qualitative ion ratio Property, quota ion area external standard method is carried out quantitatively.
Edible Semen Oryzae the most according to claim 1 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: use liquid phase Organophosphor in chromatograph/concatenation mass spectrometric determination rice sample, organic nitrogen, carbamate chemicals residual amount step as follows:
1. extract
Edible rice dry sample, weighs the size-reduced rice sample of 5.0g, is placed in 250mL plastic centrifuge tube, adds 25.0mL and steams Distilled water, stands 30min；Add 25.0ml acetonitrile, high speed dispersor is homogenized 2min, adds 10g anhydrous magnesium sulfate and 1g chlorine Changing sodium, be homogenized 1 minute in low speed dispersion machine, centrifugal force is 2500g, centrifugal 3min, makes acetonitrile and aqueous phase layering；
2. purify
Pipette 4.0ml upper strata acetonitrile solution in 15ml graduated centrifuge tube, purify, to be measured；
3. instrument condition
Chromatographic condition is as follows:
Chromatographic column: ZORBAX SB C18 (100mm × 2.1mm, 1.8 μm)；
Column temperature: 55 DEG C；
Mobile phase A: the 5mmol/L ammonium acetate solution containing 0.1% formic acid；Mobile phase B: acetonitrile；
Flow velocity: 0.3mL/min；
Mass Spectrometry Conditions is as follows:
Ion source: ESI；
Capillary voltage: 4kV；
Nitrogen flow rate: 10L/min；
Mass spectrum acquisition rate: 500ms/cycle；
Nebulizer pressure: 35psi；
Dry temperature: 350 DEG C；
4. sample determination
By the instrument condition in 3. to standard working solution and sample solution equal-volume sample introduction, according to retention time and qualitative ion and Quota ion and qualitative ion ratio carry out qualitative, and quota ion area external standard method is carried out quantitatively；
5. result calculates
In sample, tested pesticide concentration is in terms of mass fraction W, and numerical value, milligrams per kilogram to represent, is calculated by following equation:
W = A 1 × C × V 2 × V A × V 1 × V 4 V 3 × m
V1-standard specimen sampling volume, μ l；
V2-sample feeding volume, μ l；
A-standard specimen peak area；
A1-sample peak area；
M-sample quality (g)；
V3-solvent adds volume (ml)；
V4-point take solvent volume (ml)；
V-constant volume (ml).
Edible Semen Oryzae the most according to claim 1 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: step (3) In, the step of the heavy metal cadmium content in employing graphite oven atomic absorption detection edible rice is as follows:
1. prepared by sample
Removing the foreign material in rice sample, with quartering division to 50g after mixing, ground at least 98% passes through aperture The sieve of 0.180mm, standby after mixing；
2. Specimen eliminating
Weigh rice sample 0.5g to be placed in digester, add 5mL concentrated nitric acid, place 15min, build sealing lid, put microwave into In digestion system, rotate rotating disk 1min, clear up；After clearing up completely when screen instruction temperature is less than 50 DEG C, open microwave Clear up the door of instrument, the most slowly unclamp explosion-proof membrane cover to discharge pressure, take off temperature sensor, open sealing lid, by digestion solution Transfer constant volume, in 25mL volumetric flask, mix to be measured；Do reagent blank simultaneously；
3. Specification Curve of Increasing
Utilize the automatic dilution function of graphite furnace automatic sampler, make it automatically that the top mark aqueous standard method of cadmium element is bent Line, and add corresponding matrix modifier；Set the condition of instrument；Input relevant parameter, and design the concentration of standard curve Gradient；Draw standard curve；
4. calculate
X=(c-c0) × V × 1000/m × 1000 × 1000
In formula: each constituent content, mg/kg in X-sample；
C treatments of the sample liquid measures concentration, ng/mL；
C0 sample blank Digestive system concentration, ng/mL；
V treatments of the sample liquid cumulative volume, mL；
M-sample quality, g.
Edible Semen Oryzae the most according to claim 2 and the quality grading method of edible Semen oryzae sativae, it is characterised in that: according to inspection Chalkiness degree, edible quality, persticide residue and the heavy metal cadmium content recorded, carries out quality grading, specifically to edible rice As follows:
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CN113776993A (en) * 2021-07-28 2021-12-10 深圳市麦稻智联科技有限公司 Rice online detection system, detection method and detection equipment
CN114486877B (en) * 2020-10-23 2024-01-19 合肥美亚光电技术股份有限公司 Rice quality detection method, rice quality detection device and storage medium

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CN110147056A (en) * 2019-05-16 2019-08-20 珠海格力电器股份有限公司 Cooking control method, electric rice pot controller, electric cooker, terminal and system
CN110147056B (en) * 2019-05-16 2021-07-06 珠海格力电器股份有限公司 Cooking control method, electric cooker control device, electric cooker, terminal and system
CN114486877B (en) * 2020-10-23 2024-01-19 合肥美亚光电技术股份有限公司 Rice quality detection method, rice quality detection device and storage medium
CN113776993A (en) * 2021-07-28 2021-12-10 深圳市麦稻智联科技有限公司 Rice online detection system, detection method and detection equipment

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