CN101598707B - Method for detecting various pesticide residue in oil-containing food - Google Patents
Method for detecting various pesticide residue in oil-containing food Download PDFInfo
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Abstract
The invention discloses a method for detecting various pesticide residue in oil-containing food, which is implemented by adding water and acetone-normal hexane mixed solution into the oil-containing samples followed by extracting and GPC purification, adopting acetone-cyclohexane as the mobile phase, Shodex EV-2000 as the separation column, reduced pressure concentrating the respectively collected liquid to be dry according to the different peak times, dissolving the residue with methylbenzene-acetonitrile and rinsing ENVI-Carb/LC-NH2 solid phase extraction column with the methylbenzene-acetonitrile, leading the residue methylbenzene-acetonitrile solvent to pass the column and collect, rinsing with methylbenzene-acetonitrile, merging and collecting the rinsing solution, reduced pressure concentrating to be nearly dry, blowing dry with nitrogen, then dissolving with acetone-normal hexane, filtering with film, and detecting with GC/MS. Based on the principle of gel permeation chromatograph purification, the invention realizes separating the pesticide residue in oil-containing food from macromolecule fat, can fast realize separating the pesticide residue from fat and other macromolecule interfering substances, can well reduce detection limit, and achieve exact result of analysis and detection of pesticide residue in high oil-containing food.
Description
Technical field
The invention belongs to the food inspection technical field, especially relate to the residual detection method of Multiple Pesticides in a kind of oil-containing food.
Background technology
Along with the enforcement of Japanese positive list, various agricultural product limit standards are more and more lower, and the ten minutes that export situation becomes is severe.Particularly after Japan's " malicious dumpling " incident, the detection of residues of pesticides is also paid attention to by everybody gradually in the high food of fat contents such as of animal or plant nature.Past is because oil-containing food matrix is complicated, the restriction of instrument and equipment etc. simultaneously, and the good method of neither one can detect the residues of pesticides in the oil-containing food all the time.
Traditional purification method generally adopts liquid-liquid extraction or SPE to purify in food inspection.Liquid-liquid extraction consumption quantity of solvent is big, and is prone to form emulsion, operates comparatively loaded down with trivial details.Solid phase extraction Florisil post absorption commonly used lipid impurity is used low polar solvent drip washing then, is the method that analysis organochlorine, pyrethrin pesticide are used always.But, adopt methods such as conventional liquid-liquid extraction, SPE purification can not grease be removed, and operation steps is complicated for containing the higher complex matrices of grease.
Summary of the invention
The objective of the invention is to improve the deficiency of prior art and provide a kind of based on the gel permeation chromatography cleaning principle realized that but residues of pesticides in the oil-containing food are separated the separating of big molecule interfering materials such as Rapid Realization remains of pesticide and grease, can be good at reducing detection limit with big molecule grease, the analysis, testing result of satisfying residues of pesticides in the high oil-containing food residual detection method of Multiple Pesticides in the oil-containing food accurately.
The objective of the invention is to realize like this, the residual detection method of Multiple Pesticides in a kind of oil-containing food is characterized in that this method may further comprise the steps:
A, extraction: be that the oil samples that contains to be checked is added water, add acetone-normal hexane mixed liquor and extract;
B, GPC purify: moving phase adopts acetone-cyclohexane, and separating column is ShodexEV-2000, collects respectively according to the difference of appearance time, is evaporated to the liquid of collecting dried, and residue dissolves with toluene-acetonitrile;
C, ENVI-Carb/LC-NH2SPE column purification: wash the ENVI-Carb/LC-NH2 post with toluene-acetonitrile pre-leaching, the residue toluene-acetonitrile lysate that obtains in purifying GPC is then crossed post and is collected, with toluene-acetonitrile wash-out; Eluent merges to be collected; Be evaporated near doing, nitrogen dries up, and uses acetone-n-hexane dissolution then; Filtering membrane, air feed phase chromatography-mass spectroscopy detect to be used;
D, GC/MS detect:
Instrument condition: carrier gas: the helium of purity 99.999%; Chromatographic column: DB-17ms, 30m * 0.25mm * 0.25 μ m; Injector temperature: 250 ℃, shunt mode not; The column temperature program: 60 ℃ of initial temperatures, keep 1min, with 25 ℃/min, be warming up to 150 ℃, be warming up to 280 ℃ with 4.5 ℃/min again, at last with 10 ℃/min, be warming up to 300 ℃, keep 10min; Column flow rate: 1.1mL/min; Sample size: 2 μ L; Chromatography-mass spectroscopy interface temperature: 280 ℃; 230 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature; Ionization mode: electron bombard pattern (EI); Electron energy: 70eV; Mass Spectrometer Method mode: select the ion monitoring pattern.
Described extraction is to take by weighing the oil samples 10.0g that contains to be measured in the 100mL centrifuge tube, adds 10mL water, fully adds the hexane acetone volume ratio behind the mixing and be 1: 2 mixed liquor 50mL; Fierce concussion 1min; The centrifugal 5min of 3000r/min behind the ultrasonic Extraction 15min, supernatant liquor cross and are covered with a small amount of anhydrous sodium sulfate funnel, collect and filtrate in 250mL pyriform bottle; Residue extracts with the 30mL normal hexane again; Merging filtrate, 40 ℃ are evaporated to driedly, and it is 2: 8 mixed liquor dissolving that residue uses 10mL hexane acetone volume ratio.
It is that moving phase employing acetone cyclohexane volume ratio is 2: 8 a mixed liquor that described GPC purifies, and flow velocity is 5mL/min, sampling volume 5mL; Separating column:: Shodex EV-2000; In gel permeation chromatography, confirm collection time period according to standard sample of pesticide, collect respectively, transfer to the liquid of collecting in the 250mL pyriform bottle at the GPC appearance time; Be evaporated to driedly under 40 ℃, it is 1: 3 mixed liquor dissolving that residue uses 2mL toluene acetonitrile volume ratio.
Described ENVI-Carb/LC-NH2SPE column purification is that to use 10mL toluene acetonitrile volume ratio be that the ENVI-Carb/LC-NH2 post is washed in 1: 3 mixed liquor pre-leaching; Toluene-acetonitrile the lysate of the 2mL residue that obtains in purifying GPC is then crossed post and is collected; 20mL toluene acetonitrile volume ratio is 1: 3 a mixed liquor wash-out, and the eluent merging is collected in the 50mL eggplant-shape bottle, and 40 ℃ are evaporated near doing; Nitrogen dries up; Use 2.00mL hexane acetone volume ratio is 1: 1 mixed liquor dissolving, crosses 0.45 μ m filter membrane, and air feed phase chromatography-mass spectroscopy detects to be used.
The present invention is based on the gel permeation chromatography cleaning principle and realized that residues of pesticides are separated with big molecule grease in the oil-containing food; Set up the method for many residues of pesticides in the GC/MS detection oil-containing food; Method adopts the ultrasonic concussion of hexane acetone to extract, and, ENVI-Carb/LC-NH2SPE concentrated through the GPC oil removing further purifies, and finally through GC/MS residues of pesticides in the high oil-containing food detected; Experiment is through verifying that to 65 kinds of agricultural chemicals the recovery is all 70%～120%; But separating of big molecule interfering material such as the inventive method Rapid Realization remains of pesticide and grease, and can be good at reducing detection limit, satisfying the analysis of residues of pesticides in the high oil-containing food, the inventive method minimum detectability is 0.02mg/kg.
The present invention mainly adopts GPC that oil-containing food is carried out oil removing, simultaneously itself and GC/MS coupling is applied to the multi-residue analysis of agricultural chemicals in meat and the oil-containing food such as height such as conditioning food grade.The present invention has following characteristics:
1, clean-up effect:
Among the present invention its ultimate principle of the gel permeation chromatography of using be: with the porous gel in different apertures dress post; The cyclohexane of different proportionings and acetone are as eluant, eluent; According to porous gel the exclusion effect of different sized molecules is separated; First drip washing such as macromolecular grease, pigment (chlorophyll, xenthophylls), alkaloid, polymkeric substance are come out, and relative molecular masses such as agricultural chemicals are less, and back drip washing goes out.The column packing of GPC method and separated sample have no interaction, lean on the size of molecule self to separate fully.This separate mode of size has by volume determined the GPC technology under temperate condition, to carry out, because there is not reversible adsorption, so each is applicable to sample that GPC separates wash-out fully, and can obtain extraordinary purification.GPC can remove big molecule chaff interference, is applicable to more extensively, complicated more matrix.
With fried potato is example, adopts GPC to purify, and obtains its purification separation time diagram 1; Through being collected liquid, 0～11.5min, 11.5～37.0min and three time periods of 37.0～40.0min among Fig. 1 carry out weighing behind the evaporate to dryness respectively; The difference that obtains is heavy to be found with the extraction mass ratio; About 98% impurity flows out at 0～11.5min, and visible GPC is very obvious to big molecule oil separation effect; Find also in the experimentation that some pigments and target compound delivery time are overlapping, GPC can't further purify; We consider to have adopted the ENVI-Carb/LC-NH2SPE post further to purify again for this reason, and the result shows through after the above two steps purification, disturbs obviously in the testing process and reduce; Fig. 2 has improved detection sensitivity for sample chromatogram figure before purifying, Fig. 3 for purifying back sample chromatogram figure simultaneously; Reduce false-positive probability, realized how residual, high-sensitivity analysis.
2, the accuracy of method, precision and detection limit
With lean meat is example, adds 0.02mg/kg, 0.04mg/kg, 0.08mg/kg standard sample of pesticide respectively and does recovery, and each contents level repeats 3 times; The average recovery rate of resulting various agricultural chemical compounds and relative standard deviation: when the interpolation level in 0.02～0.08mg/Kg scope; The agricultural chemicals recovery is 70%～110%, and relative standard deviation is 0.7%～20.0%, n=3; The recovery and relative standard deviation all meet agricultural residual detection requirement, and the agricultural chemicals minimum detectability is 0.02mg/kg.Concrete data such as following table:
Table 1 average recovery rate and relative standard deviation n=3
Description of drawings
Fig. 1 is fried potato GPC purification separation time diagram.
Fig. 2 is fried potato sample chromatogram figure before purifying.
Fig. 3 is for purifying the fried potato sample chromatogram figure in back.
In Fig. 1: collection time period 1.: 0-11.5min, about 98% big molecular impurity is collected; Collection time period is 2.: 11.5min-37min, and acrinathrin is to the collection of Hostathion most of agricultural chemicals in the time period; Collection time period is 3.: after the 37min, and the collection of small molecular weight impurity and compound.
Embodiment
Instance 1, the residual detection method of Multiple Pesticides in a kind of oil-containing food, present embodiment is a product to be tested with fried potato; Be to take by weighing fried potato 10.0g in the 100mL centrifuge tube, add 10mL water, fully add the hexane acetone volume ratio behind the mixing and be 1: 2 mixed liquor 50mL; Fierce concussion 1min, the centrifugal 5min of 3000r/min behind the ultrasonic Extraction 15min, supernatant liquor cross and are covered with a small amount of anhydrous sodium sulfate funnel; Collection is filtrated in 250mL pyriform bottle, and residue extracts with the 30mL normal hexane again, merging filtrate; 40 ℃ are evaporated to driedly, and it is 2: 8 mixed liquor dissolving that residue uses 10mL acetone cyclohexane volume ratio; Moving phase employing acetone cyclohexane volume ratio is 2: 8 a mixed liquor, and flow velocity is 5mL/min, sampling volume 5mL; Separating column:: Shodex EV-2000; In gel permeation chromatography, confirm collection time period according to standard sample of pesticide, collect respectively, transfer to the liquid of collecting in the 250mL pyriform bottle at the GPC appearance time; Be evaporated to driedly under 40 ℃, it is 1: 3 mixed liquor dissolving that residue uses 2mL toluene acetonitrile volume ratio; The ENVI-Carb/LC-NH2SPE column purification is that to use 10mL toluene acetonitrile volume ratio be that the ENVI-Carb/LC-NH2 post is washed in 1: 3 mixed liquor pre-leaching; Toluene-acetonitrile the lysate of the 2mL residue that obtains in purifying GPC is then crossed post and is collected; 20mL toluene acetonitrile volume ratio is 1: 3 a mixed liquor wash-out, and the eluent merging is collected in the 50mL eggplant-shape bottle, and 40 ℃ are evaporated near doing; Nitrogen dries up; Use 2.00mL hexane acetone volume ratio is 1: 1 mixed liquor dissolving, crosses 0.45 μ m filter membrane, and air feed phase chromatography-mass spectroscopy detects to be used; GC/MS detects the instrument condition that is to use: carrier gas: the helium of purity 99.999%; Chromatographic column: DB-17ms, volume 30m * 0.25mm * 0.25 μ m; Injector temperature: 250 ℃, shunt mode not; The column temperature program: 60 ℃ of initial temperatures, keep 1min, with 25 ℃/min, be warming up to 150 ℃, be warming up to 280 ℃ with 4.5 ℃/min again, at last with 10 ℃/min, be warming up to 300 ℃, keep 10min; Column flow rate: 1.1mL/min; Sample size: 2 μ L; Chromatography-mass spectroscopy interface temperature: 280 ℃; 230 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature; Ionization mode: electron bombard pattern; Electron energy: 70eV; Mass Spectrometer Method mode: select ion monitoring pattern-SIM.
The fried potato of present embodiment sample is in first being processed, and raw material has the β-benzene hexachloride of low concentration to detect, and the value of detecting is 0.024mg/kg, and the employing method is GB/T 5009.146.-2003, agricultural residual drug type: benzene hexachloride-organic chlorine agriculture chemicals.Detect the result: according to the present embodiment detection method, fried potato is carried out check and analysis, β-benzene hexachloride value of detecting: 0.020mg/kg, according to GB/T 5009.146-2003 to fried potato check and analysis, β-benzene hexachloride value of detecting: ND.Above-mentioned instance explanation, fried potato and first being processed after the processing do not have significant difference on the result, explain that this method has obtained a reasonable purification with quantitative.
Instance 2, the residual detection method of Multiple Pesticides in a kind of oil-containing food, present embodiment is product to be tested with the cod; Be to take by weighing cod 10.0g in the 100mL centrifuge tube, add 10mL water, fully add the hexane acetone volume ratio behind the mixing and be 1: 2 mixed liquor 50mL; Fierce concussion 1min, the centrifugal 5min of 3000r/min behind the ultrasonic Extraction 15min, supernatant liquor cross and are covered with a small amount of anhydrous sodium sulfate funnel; Collection is filtrated in 250mL pyriform bottle, and residue extracts with the 30mL normal hexane again, merging filtrate; 40 ℃ are evaporated to driedly, and it is 2: 8 mixed liquor dissolving that residue uses 10mL acetone cyclohexane volume ratio; Moving phase employing acetone cyclohexane volume ratio is 2: 8 a mixed liquor, and flow velocity is 5mL/min, sampling volume 5mL; Separating column:: ShodexEV-2000; In gel permeation chromatography, confirm collection time period according to standard sample of pesticide, collect respectively, transfer to the liquid of collecting in the 250mL pyriform bottle at the GPC appearance time; Be evaporated to driedly under 40 ℃, it is 1: 3 mixed liquor dissolving that residue uses 2mL toluene acetonitrile volume ratio; The ENVI-Carb/LC-NH2SPE column purification is that to use 10mL toluene acetonitrile volume ratio be that ENVI ENVI-Carb/LC-NH2 post is washed in 1: 3 mixed liquor pre-leaching; The toluene acetonitrile lysate of the 2mL residue that obtains in purifying GPC is then crossed post and is collected; 20mL toluene acetonitrile volume ratio is 1: 3 a mixed liquor wash-out, and the eluent merging is collected in the 50mL eggplant-shape bottle, and 40 ℃ are evaporated near doing; Nitrogen dries up; Use 2.00mL hexane acetone volume ratio is 1: 1 mixed liquor dissolving, crosses 0.45 μ m filter membrane, and air feed phase chromatography-mass spectroscopy detects to be used; GC/MS detects the instrument condition that is to use: carrier gas: the helium of purity 99.999%; Chromatographic column: DB-17ms, volume 30m * 0.25mm * 0.25 μ m; Injector temperature: 250 ℃, shunt mode not; The column temperature program: 60 ℃ of initial temperatures, keep 1min, with 25 ℃/min, be warming up to 150 ℃, be warming up to 280 ℃ with 4.5 ℃/min again, at last with 10 ℃/min, be warming up to 300 ℃, keep 10min; Column flow rate: 1.1mL/min; Sample size: 2 μ L; Chromatography-mass spectroscopy interface temperature: 280 ℃; 230 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature; Ionization mode: electron bombard pattern; Electron energy: 70eV; Mass Spectrometer Method mode: select ion monitoring pattern-SIM.
The agricultural residual drug type that present embodiment detects: Japan's 57 organophosphorus insecticides of being open to the custom, result: all do not detect.Mark-on reclaims: add the 0.2mg/kg standard items and do recovery, establish 3 parallel, analyte recovery 75%-110%, relative standard deviation 2.8%～19.8%n=3, data are seen table 2.
Table 2. average recovery rate and relative standard deviation n=3
Above-described instance only is that specific embodiments of the invention is described, and is not scope of the present invention is limited.
Claims (1)
1. the residual detection method of Multiple Pesticides in the oil-containing food is characterized in that this method may further comprise the steps:
A, extraction: be to take by weighing the oil samples 10.0g that contains to be measured in the 100mL centrifuge tube, add 10mL water, fully add acetone and normal hexane volume ratio behind the mixing and be 1: 2 mixed liquor 50mL; Fierce concussion 1min; The centrifugal 5min of 3000r/min behind the ultrasonic Extraction 15min, supernatant liquor cross and are covered with a small amount of anhydrous sodium sulfate funnel, collect and filtrate in 250mL pyriform bottle; Residue extracts with the 30mL normal hexane again; Merging filtrate, 40 ℃ are evaporated to driedly, and it is that 2: 8 mixed liquor dissolves that residue uses 10mL acetone and cyclohexane volume ratio;
B, GPC purify: be that moving phase employing acetone and cyclohexane volume ratio are 2: 8 mixed liquor, flow velocity is 5mL/min, sampling volume 5mL; Separating column: Shodex EV-2000; Confirm collection time period according to standard sample of pesticide appearance time in gel permeation chromatography, collect respectively, transfer to the liquid of collecting in the 250mL pyriform bottle; Be evaporated to driedly under 40 ℃, it is that 1: 3 mixed liquor dissolves that residue uses 2mL toluene and acetonitrile volume ratio;
C, ENVI-Carb/LC-NH2 SPE column purification: be that to use 10mL toluene and acetonitrile volume ratio be that the ENVI-Carb/LC-NH2 post is washed in 1: 3 mixed liquor pre-leaching; The toluene of the 2mL residue that obtains in purifying GPC then and the lysate that the acetonitrile volume ratio is 1: 3 are crossed post and are collected; 20mL toluene and acetonitrile volume ratio are 1: 3 mixed liquor wash-out, and the eluent merging is collected in the 50mL eggplant-shape bottle, and 40 ℃ are evaporated near doing; Nitrogen dries up; Use 2.00mL acetone and normal hexane volume ratio are 1: 1 mixed liquor dissolving, cross 0.45 μ m filter membrane, and air feed phase chromatography-mass spectroscopy detects to be used;
D, GC/MS detect:
Instrument condition: carrier gas: the helium of purity 99.999%; Chromatographic column: DB-17ms, 30m * 0.25mm * 0.25 μ m; Injector temperature: 250 ℃, shunt mode not; The column temperature program: 60 ℃ of initial temperatures, keep 1min, with 25 ℃/min, be warming up to 150 ℃, be warming up to 280 ℃ with 4.5 ℃/min again, at last with 10 ℃/min, be warming up to 300 ℃, keep 10min; Column flow rate: 1.1mL/min; Sample size: 2 μ L; Chromatography-mass spectroscopy interface temperature: 280 ℃; 230 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature; Ionization mode: electron bombard pattern; Electron energy: 70eV; Mass Spectrometer Method mode: select the ion monitoring pattern.
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