CN105510506A - Method for GC-MS/MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables - Google Patents
Method for GC-MS/MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables Download PDFInfo
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Abstract
The invention discloses a method for GC-MS/MS (gas chromatography tandem mass spectrometry) determination of penflufen remains in fruits and vegetables. Penflufen remains in a sample is extracted by acetonitrile or an acetonitrile solution containing 1% acetic acid, the extracting solution is dispersed and purified by an ethylenediamine-N-propylsilane (PSA) and octadecylsilan bonded phase (C18) substrate, GC-MS/MS detection is performed, a corrected standard work curve is built by adopting a blank substrate solution without to-be-detected pesticide, and quantification is performed with an external standard method. The method has the average recovery rate being 84.3%-90.6%, the average relative standard deviation (RSD) being 5.0%-8.0%, and the detection limit lower than 0.032 microgram/kilogram, and has the advantages of simple operation, rapidness, high sensitivity, good repeatability, high qualitative and quantitative precision, thereby meeting the technical requirements for safety detection of corresponding products in the USA, EU, Japan, and other countries, and providing strong technical support for ensuring Chinese food safety and export abroad trade healthy development.
Description
Technical field
The present invention relates to a kind of method that GC-MS/MS measures fluorine azoles bacterium aniline residue in fruits and vegetables, be more particularly the method adopting gas chromatography tandem mass spectrum (GC-MS/MS) qualitative, quantitative to measure fluorine azoles bacterium aniline content residual in vegetables and fruit, belong to the determination techniques field of persticide residue.
Background technology
Fluorine azoles bacterium aniline is the succinate dehydrogenase inhibitors series bactericidal agent developed by BASF AG, common name: penflufen; Test code number: BYF14182; Fluoro-1, the 3-dimethyl-1H-pyrazole-4-carboxamide of chemical name: N-[2-(1,3-dimethylbutyl) phenyl]-5-; Outward appearance: gray powdery solid; Fusing point: 111 DEG C; Boiling point: decompose before boiling point; Decomposition temperature: 320 DEG C; Vapor pressure: 1.2 × 10
-6pa (25 DEG C); Partition factor: KowlogP=3.3 (20 DEG C, pH=7); Henry's constant: 1.05 × 10
-5pam
3mol-1 (25 DEG C).Solubleness: the solubleness in water is 10.9mg/L (20 DEG C); Solubleness in normal hexane is 1.6g/L, is 62g/L in toluene, is 139g/L in acetone, is 126g/L in methyl alcohol, is 96g/L in ethyl acetate, is 162g/L (being 20 DEG C above) in dimethyl sulfoxide; CAS accession number: 494793-67-8.Relative molecular mass 317.41; Molecular formula C
18h
24fN
3o, chemical structural formula is:
Fluorine azoles bacterium aniline is another pyrazole amide series bactericidal agent of Beyer Co., Ltd's exploitation, applies for a patent, is mainly used in Seed Treatment, have excellent activity to various plants disease fungus in 2006.This germifuge is succinate dehydrogenase (SDH) inhibitor, mainly acts on respiratory chain electron transmission Complex II, blocks energetic supersession.Seed after treatment can absorb fluorine azoles bacterium aniline in germination process, and is transmitted to other positions of plant by xylem, thus plays the effect of cover crop.Fluorine azoles bacterium aniline is a seed treatment fungicides, for seeds such as potato, corn, paddy rice, cotton, wheat, barley, clover, vegetables, beans and rapes, can to prevent and treat kind pass, basidiomycetes that soil passes and sac fungus disease, mainly contain the disease such as black scurf of potato, wheat sharp eyespot, rice sheath blight disease, sclerotinia rot of colza, loose smut of wheat, the bunt of wheat, corn southern leaf blight that rhizoctonia (Rhizoctoniaspp.) and ustilagin (Ustilagospp.) etc. cause.Can be composite with prothioconazoles, metalaxyl, clothianidin, oxime bacterium ester etc., not only can prevention and elimination of disease and pests, can also delaying drug resistance producing and developing.Fluorine azoles bacterium aniline obtained the registration of the first whole world in 2011 in Britain, within 2012, obtained its registration approval again at America & Canada, obtained registration, have very wide application prospect in Australia and a lot of country.
Along with the registration of fluorine azoles bacterium aniline, popularization and use, the country such as U.S. as China's main exit market has formulated its maximum maximum permission quantity (MRL) in the food agricultural product such as veterinary antibiotics, Cereals and livestock products, on May 14th, 2012, the newly-increased residue limits requirement to agricultural chemicals penta benzene pyrrole bacterium amine (Penflufen) of the U.S., residue limits requires to provide as follows:
If European Union, Japan and other countries regulation field use agricultural chemicals not register in this country, when not formulating corresponding residue limits standard, the food agricultural product being exported to its country comprise " uniform limit " that residue limits in the animal derived foods such as livestock meat all carries out 0.01mg/L.
Present stage, less to the research of fluorine azoles bacterium aniline residue quantity measuring method, the detection method of report is mainly fluorine azoles bacterium aniline residue detection method in vegetables and fruit, these detection methods all adopt Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) to measure the detection method of fluorine azoles bacterium aniline residue amount in vegetables and fruit, using LC-MS/MS to measure food Residual Pesticides in Farm Produce has fast, easy, sensitivity advantages of higher, but due to its price costly, a lot of testing agency, enterprise or scientific research institutions do not configure this instrument or configuration number of units is less, during due to different compounds employing LC-MS/MS detection, different mobile phases or chromatographic column need be used, such needs constantly change chromatographic column, mobile phase also expends the long time and balances system, this constrains the application of LC-MS/MS to a certain extent.Use gas chromatography tandem mass spectrum (GC-MS/MS) to analyze food Residual Pesticides in Farm Produce and there is the advantages such as quick, easy, highly sensitive, selectivity is strong, the multi-residue analysis of hundreds of kind agricultural chemicals can be realized, but have no the report of the GC-MS/MS detection method of fluorine azoles bacterium aniline residue amount in food agricultural product up to now, therefore set up easy, quick, accurate, durable, can accurately in qualitative and quantitative analysis vegetables and fruit the GC-MS/MS detection method of fluorine ether bacterium acid amides residual quantity significant.
Summary of the invention
The object of this invention is to provide a kind of method that GC-MS/MS measures fluorine azoles bacterium aniline residue in fruits and vegetables.
For realizing above object, the technical solution adopted in the present invention is: a kind of GC-MS/MS measures the method for fluorine azoles bacterium aniline residue in fruits and vegetables, comprises the steps:
(1) extract
Take sample in tool plug centrifuge tube, add acetonitrile or extract 1min containing the acetonitrile solution homogeneous of 1% acetic acid, add the one in sodium chloride or sodium acetate and anhydrous magnesium sulfate, centrifugal after vibration.
(2) purify
Pipette sample extracting solution supernatant in centrifuge tube, add Dispersive solid phase extraction agent, vortex oscillation, centrifugal, draw after a certain amount of scavenging solution nitrogen dries up, dissolve constant volume with acetone/normal hexane mixed solvent that volume ratio is 1/1, after crossing film, treat that gas chromatography tandem mass spectrum (GC-MS/MS) detects.
(3) preparation of standard working solution
During by the same kind matrix blank sample of not fluorine-containing azoles bacterium aniline by above-mentioned steps (1), (2) process, obtain sample extraction purification residue, add appropriate solvent and standard solution, vortex mixes, and is mixed with the fluorine azoles bacterium aniline series hybrid standard working fluid of at least 3 concentration.
(4) gas chromatography tandem mass spectrometry (GC-MS/MS) measures
The standard working solution of each concentration gradient in step (3) is carried out GC-MS/MS mensuration, with the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain standard working curve; Under the same conditions the sample liquid after purification in step (2) is injected GC-MS/MS to measure, record the chromatographic peak area of fluorine azoles bacterium aniline in sample liquid, substitute into standard working curve, obtain fluorine azoles bacterium aniline content in sample liquid, then the Mass Calculation of sample representated by liquid obtains fluorine azoles bacterium aniline residue amount in sample per sample; If fluorine azoles bacterium aniline residue amount exceedes the range of linearity upper limit in upper machine solution, with constant volume solvent, upper machine solution concentration need be diluted within the range of linearity.
Step (1) if in sample dehydrated vegetables and fruit, need sample weighting amount be reduced, and add suitable quantity of water and fully infiltrate.
Add sodium chloride when adopting acetonitrile to extract in step (1) to saltout, add sodium acetate when adopting the acetonitrile solution containing 1% acetic acid to extract and saltout; A certain amount of water need be added when the sample of moisture content less is saltoutd.
The agent of step (2) mesostroma dispersive solid-phase extraction is by anhydrous magnesium sulfate, C
18with PSA composition, anhydrous magnesium sulfate, C in every milliliter of extract
18150mg, 50mg and 25mg is respectively with PSA addition.
In step (4), GC conditions is: chromatographic column: HP-5MS capillary chromatographic column, column length 30m, internal diameter 0.25mm, thickness 0.25 μm; Injector temperature 250 DEG C; Carrier gas: He, not shunt mode sample introduction, sample size: 1 μ L; Constant current mode, flow velocity 1.2mL/min; Heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C, then rises to 220 DEG C with the speed of 2 DEG C per minute, then rise to 280 DEG C with the speed of 20 DEG C per minute with the speed of 20 DEG C per minute, keeps 10min; Transmission line temperature: 290 DEG C.
In step (4), Mass Spectrometry Conditions is: ionization pattern: electron impact ionization (EI, 70eV); Ion source temperature 280 DEG C; Collision gas: argon gas; Multiple-reaction monitoring scan mode MRM, monitoring parameter is:
When measuring sample liquid and extraction standard working solution in step (4), if sample liquid Pesticides chromatographic peak retention time agricultural chemicals retention time corresponding to standard solution is consistent, and in the sample mass spectrogram after background correction, selected ion all occurs, and abundance of ions than with the abundance of ions of standard solution than consistent, then can judge to exist in sample liquid this agricultural chemicals; If above-mentioned two conditions can not meet simultaneously, then judge not containing this kind of agricultural chemicals.
Beneficial effect of the present invention is:
The present invention utilizes dispersive solid-phase extraction technology, establish sample-pretreating method that is easy, that also can effectively avoid sample mesostroma to disturb fast, this pre-treating method is applied to the qualitative confirmation of fluorine azoles bacterium aniline and quantitatively detection in vegetables and fruit in conjunction with GC-MS/MS, average recovery rate is 84.3% ~ 90.6%, average relative standard's deviation (RSD) is 5.0% ~ 8.0%, detection limit, lower than 0.032 μ g/kg, has easy and simple to handle, quick, accurate, highly sensitive and reproducible advantage.The U.S., European Union, Japan and other countries being met to the technical requirement of corresponding product safety detection, providing strong technical support for ensureing that our people's food security and export abroad trade develop in a healthy way.
Accompanying drawing explanation
Fig. 1 is the Selective ion mode chromatogram of the 5ng/mL fluorine azoles bacterium aniline mark liquid be added in blank apple matrix.
Fig. 2 is the Selective ion mode chromatogram of the apple blank sample of not fluorine-containing azoles bacterium aniline.
The fluorine azoles bacterium aniline standard working curve that Fig. 3 is is substrate preparation with the apple blank sample of not fluorine-containing azoles bacterium aniline.
Embodiment
Now with following embodiment, the present invention is described, but is not limit the scope of the invention.
The instrument used in embodiment and reagent
T18Basic homogenizer (IKA, Germany); 5810R hydro-extractor (Eppendorf, Germany); MS3 basic model vortex mixer (IKA, Germany); 7890N gas chromatography-5977C mass spectrometer (Agilent, USA); Primary secondary amine (PSA) adsorbent (40 ~ 60 μm), octadecylsilane Bonded Phase (C
18) cleanser (40 ~ 60 μm) is all purchased from Anjelen Sci. & Tech. Inc of the U.S..
Reagent: acetonitrile, acetone, normal hexane (HPLC level, Merke, Germany); Acetic acid (HPLC level, CNW, Germany); Anhydrous magnesium sulfate, sodium chloride and sodium acetate are pure for analyzing, all purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
Standard substance: purity 99.5%, purchased from German Dr.Ehrenstorfer company.
Embodiment 1: the detection of fluorine azoles bacterium aniline residue amount in apple
(1) sample pre-treatments
Taking apple 10.0g through fully mixing in 50mL centrifuge tube, accurately adding 20mL acetonitrile, homogeneous extracts 1min, adds 3g anhydrous magnesium sulfate and 2g sodium chloride, after vortex 1min, and the centrifugal 5min of 7000r/min.After centrifugal, get 6mL acetonitrile extract and be transferred to 900mg anhydrous magnesium sulfate, 300mgC are housed
18with in the centrifuge tube of 150mgPSA, the centrifugal 5min of vortex 1min, 5000r/min.Get 1mL supernatant in nitrogen blowpipe, dry up in 40 DEG C of nitrogen, add acetone/normal hexane mixed solvent dissolved residue that volume ratio is 1/1, after vortex mixed film, move in sample injection bottle and treat that GC-MS/MS measures.
(2) preparation of standard working solution
Accurately take 25 ± 0.1mg standard items in 25mL volumetric flask, dissolve with acetonitrile, constant volume obtains 1000.0 μ g/mL standard reserving solutions; Pipette 1.0mL standard reserving solution and be placed in 100mL volumetric flask, obtain 10.0 μ g/mL standard intermediate liquids with the acetone/normal hexane mixed solvent constant volume by volume ratio being 1/1; By the apple blank sample of not fluorine-containing azoles bacterium aniline by above-mentioned pre-treatment step process, get the blank extraction and cleaning liquid of 8mL, be concentrated into after doing, add acetone/normal hexane mixed solvent vortex dissolving that 8mL volume ratio is 1/1, be finally mixed with 1,2,5,10,20,50 μ g/L extraction standard working solutions with this solution.
(3) gas chromatography tandem mass spectrometry (GC-MS/MS) measures
The standard working solution of variable concentrations gradient is injected GC-MS/MS respectively, carries out the quantitative test of fluorine azoles bacterium aniline content with external standard method, namely with the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain standard working curve; Under the same conditions sample extracting solution is injected GC-MS/MS to measure, record the chromatographic peak area of fluorine azoles bacterium aniline in sample liquid, substitute into standard working curve, obtain fluorine azoles bacterium aniline content in sample liquid, then the Mass Calculation of sample representated by liquid obtains fluorine azoles bacterium aniline residue amount in sample per sample.
Wherein chromatographic condition is:
Chromatographic column: HP-5MS capillary chromatographic column, column length 30m, internal diameter 0.25mm, thickness 0.25 μm.
Injector temperature: 250.0 DEG C, sample introduction pattern: Splitless injecting samples, sample size: 1 μ L.
Carrier gas: He, constant current mode, flow velocity 1.2mL/min.
Stove case heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C, then rises to 220 DEG C with the speed of 2 DEG C per minute, then rise to 280 DEG C with the speed of 20 DEG C per minute with the speed of 20 DEG C per minute, keeps 10min;
Transmission line temperature: 290 DEG C.
Wherein, mass spectrometry parameters is:
Ionization pattern: electron impact ionization, i.e. EI pattern, energy 70eV.
Ion source temperature: 280 DEG C.
Collision gas: argon gas.
Scan mode: multiple-reaction monitoring (SRM) scan pattern.
MRM detected parameters is in table 1.
Table 1: the MRM detected parameters of embodiment 1
*for quota ion pair.
Qualitative Identification: at identical conditions, if sample liquid Pesticides chromatographic peak retention time agricultural chemicals retention time corresponding to standard solution is consistent, and in the sample mass spectrogram after background correction, selected ion all occurs, and abundance of ions than with the abundance of ions of standard solution than consistent, then can judge to exist in sample liquid this agricultural chemicals; If above-mentioned two conditions can not meet simultaneously, then judge not containing this kind of agricultural chemicals.
With the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain standard working curve as table 2.
The standard working curve of fluorine azoles bacterium aniline in table 2 apple bare substrate
| Title | Retention time (min) | Regression equation | Related coefficient |
| Fluorine azoles bacterium aniline | 20.15 | Y＝30053X+12919 | 0.9994 |
Recovery of standard addition and repeatability:
The fluorine azoles bacterium aniline standard solution of 10, a 20 and 200 μ g/kg3 concentration level is added in the apple of not fluorine-containing azoles bacterium aniline, add after 30min until agricultural chemicals and carry out the determination of residual amount by above-mentioned treatment step, the sample liquid volume ratio to be measured that 200 μ g/kg add concentration be 1/1 acetone/normal hexane mixed solvent measure with GC-MS/MS again after diluting 5 times.Mensuration concentration and agricultural chemicals theory are added concentration compare, obtain agricultural chemicals TIANZHU XINGNAO Capsul, each Pitch-based sphere replicate determination 6 times, obtain its relative standard deviation, measurement result is in table 3.As can be seen from Table 3, in 3 mark-on levels, the average recovery rate of fluorine azoles bacterium aniline is 84.9% ~ 90.2%, and average relative standard's deviation (RSD) is 5.0% ~ 6.6%, illustrates that the recovery of the inventive method is higher, reproducible.
The recovery of table 3 fluorine azoles bacterium aniline and repeatability (n=6)
Detection limit:
The fluorine azoles bacterium aniline matrix standard working solution of variable concentrations is injected GC-MS/MS, calculate detection limit with the cycles of concentration (cycles of concentration of apple is 0.5 times) of 3 times of signal to noise ratio (S/N ratio)s of least concentration extraction standard solution chromatographic peak and sample handling processes, detecting of fluorine azoles bacterium aniline is limited to 0.032 μ g/kg.
Embodiment 2: the detection of fluorine azoles bacterium aniline residue amount in cucumber
(1) sample pre-treatments
Take cucumber 10.0g through fully mixing in 50mL centrifuge tube, accurately add the acetonitrile solution of 20mL containing 1% acetic acid, homogeneous extracts 1min, adds 3g anhydrous magnesium sulfate, 2g sodium acetate and 2mL water, after vortex 1min, and the centrifugal 5min of 7000r/min.After centrifugal, get 6mL acetonitrile extract and be transferred to 900mg anhydrous magnesium sulfate, 300mgC are housed
18with in the centrifuge tube of 150mgPSA, the centrifugal 5min of vortex 1min, 5000r/min.Get 1mL supernatant in nitrogen blowpipe, dry up in 40 DEG C of nitrogen, add acetone/normal hexane mixed solvent dissolved residue that volume ratio is 1/1, after vortex after mixing, move in sample injection bottle and treat that GC-MS/MS measures.
(2) preparation of standard working solution
Acetone/normal hexane the mixed solvent being 1/1 by 1000 μ g/mL standard intermediate liquid solution volume ratios is diluted to 10 μ g/mL standard intermediate liquids.By the cucumber blank sample of not fluorine-containing azoles bacterium aniline by above-mentioned pre-treatment step process, get the blank extraction and cleaning liquid of 8mL, be concentrated into after doing, add acetone/normal hexane mixed solvent vortex dissolving that 8mL volume ratio is 1/1, be finally mixed with 1,2,5,10,20,50 μ g/L extraction standard working solutions with this solvent.
(3) gas chromatography tandem mass spectrometry (GC-MS/MS) measures
Operation steps, chromatogram are consistent with the mensuration of fluorine azoles bacterium aniline in above-mentioned apple sample with Mass Spectrometry Conditions.
Qualitative Identification:
Consistent with the mensuration of fluorine azoles bacterium aniline in above-mentioned apple sample.
Linear relationship:
Carry out regretional analysis with the chromatographic peak area of standard working solution to its respective concentration, obtaining standard working curve is Y=46047X+5403.6, and related coefficient is 0.9992.
Recovery of standard addition and repeatability:
The fluorine azoles bacterium aniline standard solution of 10, a 20 and 200 μ g/kg3 concentration level is added in the cucumber of not fluorine-containing azoles bacterium aniline, add after 30min until agricultural chemicals and carry out the determination of residual amount by above-mentioned treatment step, the sample liquid volume ratio to be measured that 200 μ g/kg add concentration be 1/1 acetone/normal hexane mixed solvent measure with GC-MS/MS again after diluting 5 times.Mensuration concentration and agricultural chemicals theory are added concentration compare, obtain agricultural chemicals TIANZHU XINGNAO Capsul, each Pitch-based sphere replicate determination 6 times, obtain its relative standard deviation, measurement result is in table 4.As can be seen from Table 4, in 3 mark-on levels, the average recovery rate of fluorine azoles bacterium aniline is 84.3% ~ 90.6%, and average relative standard's deviation (RSD) is 6.4% ~ 8.0%, illustrates that the recovery of the inventive method is high, reproducible.
The recovery of table 4 fluorine azoles bacterium aniline and repeatability (n=6)
Detection limit:
The fluorine azoles bacterium aniline matrix standard working solution of variable concentrations is injected GC-MS/MS, calculate detection limit with the cycles of concentration (cycles of concentration of cucumber is 0.5 times) of 3 times of signal to noise ratio (S/N ratio)s of least concentration extraction standard solution chromatographic peak and sample handling processes, detecting of fluorine azoles bacterium aniline is limited to 0.019 μ g/kg.
Above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various modification that the common engineering in this area is made technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (5)
1. GC-MS/MS measures a method for fluorine azoles bacterium aniline residue in fruits and vegetables, it is characterized in that, said method comprising the steps of:
(1) extract
Take vegetables and fruit sample in tool plug centrifuge tube, add acetonitrile or extract 1min containing the acetonitrile solution homogeneous of 1% acetic acid, centrifugal after adding one in sodium chloride or sodium acetate and anhydrous magnesium sulfate vibration;
(2) purify
Pipette sample extracting solution in centrifuge tube, add Dispersive solid phase extraction agent, vortex oscillation, centrifugal, get after a certain amount of scavenging solution nitrogen dries up, dissolve constant volume with acetone/normal hexane mixed solvent that volume ratio is 1/1, after crossing film, treat that gas chromatography tandem mass spectrum (GC-MS/MS) detects;
(3) preparation of standard working solution
By the same kind matrix blank sample of not fluorine-containing azoles bacterium aniline by above-mentioned steps (1), (2) process, obtain sample extraction purification residue, add appropriate solvent and standard solution, vortex mixes, and is mixed with the fluorine azoles bacterium aniline series hybrid standard working fluid of at least 3 concentration;
(4) mensuration and result calculate
The standard working solution of each concentration gradient in step (3) is carried out GC-MS/MS mensuration, with the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain extraction standard working curve; Under the same conditions the sample liquid after purification in step (2) is injected GC-MS/MS to measure, record the chromatographic peak area of fluorine azoles bacterium aniline in sample liquid, substitute into extraction standard working curve, obtain fluorine azoles bacterium aniline content in sample liquid, then the Mass Calculation of sample representated by liquid obtains fluorine azoles bacterium aniline residue amount in sample per sample; If fluorine azoles bacterium aniline residue amount exceedes the range of linearity upper limit in upper machine solution, with constant volume solvent, upper machine solution concentration need be diluted within the range of linearity.
2. a kind of GC-MS/MS according to claim 1 measures the method for fluorine azoles bacterium aniline residue in fruits and vegetables, it is characterized in that, step (1) if in vegetables and fruit sample dehydrated sample, need sample weighting amount be reduced, and add suitable quantity of water and fully infiltrate.
3. a kind of GC-MS/MS according to claim 1 measures the method for fluorine azoles bacterium aniline residue in fruits and vegetables, it is characterized in that, sodium chloride need be added when adopting acetonitrile to extract in step (1) to saltout, sodium acetate need be added when adopting the acetonitrile solution containing 1% acetic acid to extract and saltout.
4. a kind of GC-MS/MS according to claim 1 measures the method for fluorine azoles bacterium aniline residue in fruits and vegetables, and it is characterized in that, the agent of step (2) mesostroma dispersive solid-phase extraction is by anhydrous magnesium sulfate, C
18with PSA composition, anhydrous magnesium sulfate, C in every milliliter of extract
18150mg, 50mg and 25mg is respectively with PSA addition.
5. a kind of GC-MS/MS according to claim 1 measures the method for fluorine azoles bacterium aniline residue in fruits and vegetables, it is characterized in that, in step (4), GC-MS/MS analysis condition is: chromatographic column: HP-5MS capillary chromatographic column, column length 30m, internal diameter 0.25mm, thickness 0.25 μm; Injector temperature 250.0 DEG C; Carrier gas: He, not shunt mode sample introduction, sample size: 1 μ L; Constant current mode, flow velocity 1.2mL/min; Heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C, then rises to 220 DEG C with the speed of 2 DEG C per minute, then rise to 280 DEG C with the speed of 20 DEG C per minute with the speed of 20 DEG C per minute, keeps 10min; Transmission line temperature: 290 DEG C; Ionization pattern: electron impact ionization (EI, 70eV); Ion source temperature 280 DEG C; Collision gas: argon gas; Multiple-reaction monitoring scan mode, monitoring parameter is:
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| LIU XINGANG 等: "Determination of tebuconazole, trifloxystrobin and its metabolite in fruit and vegetables by a Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method using gas chromatography with a nitrogen–phosphorus detector and ion trap mass spectrometry", 《BIOMED.CHROMATOGR.》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109001315A (en) * | 2018-07-13 | 2018-12-14 | 深圳天祥质量技术服务有限公司 | The screening test method of gourd, fruit and vegetable pesticide residue |
| CN112083116A (en) * | 2020-09-29 | 2020-12-15 | 合肥海关技术中心 | Method for measuring residual quantity of prothioconazole and metabolite thioneazole thereof in apples |
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