CN105717220A - GC-MS/MS rapid measurement method for penflufen residual amount - Google Patents

GC-MS/MS rapid measurement method for penflufen residual amount Download PDF

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CN105717220A
CN105717220A CN201610070299.7A CN201610070299A CN105717220A CN 105717220 A CN105717220 A CN 105717220A CN 201610070299 A CN201610070299 A CN 201610070299A CN 105717220 A CN105717220 A CN 105717220A
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azoles bacterium
bacterium aniline
fluorine azoles
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崔淑华
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    • G01N30/02—Column chromatography
    • 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
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Abstract

The invention discloses a GC-MS/MS rapid measurement method for the penflufen residual amount.The method is mainly used for measuring the content of residual penflufen in animal derived food high in fat content.Residual penflufen in a sample is extracted with acetonitrile in a homogeneous mode, after dispersion and purification are conducted on an extracting solution through an enhanced matrix removal (EMR) product substrate and extraction through a back extraction pipe and concentration are conducted, gas chromatography-tandem-mass spectrum (GC-MS/MS) detection is conducted, a corrected standard work curve is established through an empty substrate solution containing no to-be-measured pesticide, and external standard method quantitation is conducted.The average recovery rate of the method is 86.9-88.1%, the average relative standard deviation (RSD) is 6.6-8.4%, and the detection limit is lower than 0.010 microgram per kilogram.The method has the advantages of being easy and convenient to operate, rapid, good in impurity removal effect, high in sensitivity, strong in characteristic feature, good in repeatability and accurate in qualifying and quantifying.The technical requirements of America, European Union, Japan and other countries for safety detection on corresponding products can be met, and powerful technical support is provided for ensuring food safety of people in China and healthy development of export trades.

Description

A kind of GC-MS/MS rapid assay methods of fluorine azoles bacterium aniline residue amount
Technical field
The present invention relates to the GC-MS/MS rapid assay methods of a kind of fluorine azoles bacterium aniline residue amount, more specifically use gas Phase chromatographic tandem mass spectrum (GC-MS/MS) qualitative, quantitative measures animal muscle and the goods etc. such as Carnis Sus domestica, beef, Carnis caprae seu ovis, Carnis Gallus domesticus The method of the fluorine azoles bacterium aniline content of residual in the animal derived food that fat content is high, belongs to the determination techniques neck of persticide residue Territory.
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；Chemical name: N-[2-(1,3-dimethylbutyl) phenyl]-5-fluoro-1,3-dimethyl-1H-pyrazoles-4- Methanamide；Outward appearance: gray powdery solid；Fusing point: 111 DEG C；Boiling point: decompose before boiling point；Decomposition temperature: 320 DEG C； Vapour pressure: 1.2 × 10-6Pa(25℃)；Partition coefficient: Kow logP=3.3 (20 DEG C, pH=7)；Henry's constant: 1.05 × 10-5 Pa·m3·mol-1(25℃).Dissolubility: the dissolubility in water is 10.9mg/L (20 DEG C)；Dissolubility in normal hexane For 1.6g/L, toluene is 62g/L, acetone is 139g/L, methanol is 126g/L, ethyl acetate is 96g/L, diformazan For 162g/L (being 20 DEG C above) in sulfoxide；CAS accession number: 494793-67-8.Relative molecular mass 317.41；Point Minor C18H24FN3O, chemical structural formula is:
Fluorine azoles bacterium aniline is another pyrazole amide series bactericidal agent of Beyer Co., Ltd's exploitation, applied for a patent in 2006, mainly uses In seed treatment, various plants pathogenic fungi had excellent activity.This antibacterial is succinate dehydrogenase (SDH) inhibitor, Mainly act on respiratory chain electron transmission Complex II, block energy metabolism.Seed after treatment is permissible in germination process Absorption fluorine azoles bacterium aniline, and other positions of plant it are transmitted to by xylem, thus play the effect of cover crop.Fluorine azoles Bacterium aniline is a seed treatment fungicides, for Rhizoma Solani tuber osi, Semen Maydis, Oryza sativa L., Cotton Gossypii, Semen Tritici aestivi, Fructus Hordei Vulgaris, Herba Medicaginis, vegetable, The seed such as beans and Brassica campestris L, can prevent and treat kind of a biography, the basidiomycetes of soil biography and ascomycetes disease, mainly have rhizoctonia Black scurf of potato that (Rhizoctonia spp.) and ustilagin (Ustilago spp.) etc. cause, wheat sharp eyespot, Oryza sativa L. stricture of vagina The diseases such as rot, sclerotinia rot of colza, loose smut of wheat, the bunt of wheat, corn southern leaf blight.Can be with prothioconazoles, first Frost spirit, clothianidin, trifloxystrobin etc. are compounding, are possible not only to prevention and elimination of disease and pests, it is also possible to delaying drug resistance produces and development.Fluorine azoles bacterium Aniline obtained the registration of the first whole world in 2011 in Britain, within 2012, obtained its registration approval at America & Canada again, big in Australia Leah and a lot of country obtain registration, have the most wide application prospect.
Along with fluorine azoles bacterium aniline registration, promote and use, the country such as U.S. as China's main exit market has formulated it Maximum allowable residual quantity (MRL) in the food agricultural product such as veterinary antibiotics, Cereals and livestock products, 2012 year May 14 Day, the newly-increased residue limits requirement to pesticide penflufen-containing (Penflufen) of the U.S., residue limits requires to provide as follows:
If European Union, Japan and other countries regulation field use pesticide not register in this country, when not formulating corresponding residue limits standard, The food agricultural product being exported to its country include that in the animal derived foods such as livestock meat, residue limits all carries out the " same of 0.01mg/L Standard ".
Present stage, the research to fluorine azoles bacterium aniline residue quantity measuring method is less, and the detection method of report is mainly vegetable and water Fluorine azoles bacterium aniline residue detection method in Guo, these detection methods all use Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) to measure The detection method of fluorine azoles bacterium aniline residue amount in vegetable and fruit, uses LC-MS/MS to measure food Residual Pesticides in Farm Produce tool There is quick, easy, sensitivity advantages of higher, but due to its price costly, a lot of testing agencies, enterprise or scientific research institutions are not Configure this instrument or configuration number of units is less, when using LC-MS/MS detection due to different compounds, different flowings need to be used Mutually or chromatographic column, such needs are constantly changed chromatographic column, flowing and mutually and are expended the long time and be balanced system, this Determine to constrain in degree the application of LC-MS/MS.Gas chromatogram tandem mass spectrum (GC-MS/MS) is used to analyze food agricultural product Pesticide Residues has the advantages such as quick, easy, highly sensitive, selectivity is strong, can realize the multi-residue analysis of hundreds of kind of pesticide, 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, but up to now Have no the report of the GC-MS/MS detection method of fluorine azoles bacterium aniline residue amount in food agricultural product.Additionally, it is well known that, QuEChERS pretreatment technology has become sample-pretreating method most widely used in pesticide residue analysis, but QuEChERS side Method is primarily adapted for use in the High water cut substrate of low-fat content, such as most fruit and vegetable, energy when in the face of high fat content substrate Power is limited, it is generally required to increase normal hexane grease removal, freezing sample extracting solution goes the steps such as fat, but effect is limited.In recent years some Company is proposed enhancement mode lipid and removes patented product-Enhanced Matrix Removal, EMR-lipid, is mainly used in removing tool There is the lipid chaff interference of straight chain hydrocarbon structure, including free fatty, cholesterol, triglyceride, phospholipid etc..This product by Make matrix solid phase dispersion extractant, hydroactivated after can directly by dispersive solid-phase extraction flow process to the lipid impurities in extracting solution Being removed, the present invention applies this pre-treating method to find when purifying animal derived food, and the method is simply efficient, to lipid Matter removal effect is good, sets up the dispersion purification of EMR substrate, gas chromatogram tandem mass spectrum (GC-MS/MS) qualitative and quantitative analysis In animal derived food, the detection method of fluorine azoles bacterium aniline residue amount is significant.
Summary of the invention
It is an object of the invention to provide the GC-MS/MS rapid assay methods of a kind of fluorine azoles bacterium aniline residue amount, be mainly used in surveying Determine fluorine azoles bacterium aniline residue amount in the food agricultural product that the fat contents such as animal derived food are high.
For realizing object above, the technical solution adopted in the present invention is: the GC-MS/MS of a kind of fluorine azoles bacterium aniline residue amount Rapid assay methods, comprises the steps:
(1) extract
Weigh mixing sample in tool plug centrifuge tube in, add suitable quantity of water recovery after, be quantitatively adding acetonitrile solution homogenizing extract, be subsequently adding Sodium chloride and anhydrous magnesium sulfate, centrifugal after violent vortex 1min.
Purify
By enhancement mode lipid remove product E MR use water activation, pipette sample extracting solution in activate EMR purification pipe in, vortex 1min After, 7000r/min is centrifuged 5min, shifts whole supernatant and saltouts to the centrifuge tube equipped with anhydrous magnesium sulfate and sodium chloride, After vortex centrifugal, pipette the supernatant of certain volume, after being concentrated to dryness, molten with the acetone that volume ratio is 1/1/normal hexane mixed solvent Solve constant volume, after crossing film, treat that gas chromatogram tandem mass spectrum (GC-MS/MS) detects.
(3) preparation of standard working solution
The same kind matrix blank sample of the most fluorine-containing azoles bacterium aniline is processed by above-mentioned steps (1), (2), obtains sample extraction and purify residual Slag, adds appropriate solvent and standard solution, and vortex mixes, and is configured to the fluorine azoles bacterium aniline series standard working solution of at least 3 concentration.
(4) measure and result calculates
The standard working solution of each Concentraton gradient in step (3) is carried out GC-MS/MS mensuration, with the chromatographic peak area of standard working solution Its respective concentration is carried out regression analysis, obtains extraction standard working curve；After step (2) being purified under the same conditions Sample liquid is injected GC-MS/MS and is measured, and records the chromatographic peak area of fluorine azoles bacterium aniline in sample liquid, substitutes into extraction standard work Make curve, obtain fluorine azoles bacterium aniline content in sample liquid, then obtain in sample according to the Mass Calculation of sample representated by sample liquid Fluorine azoles bacterium aniline residue amount；If fluorine azoles bacterium aniline residue amount exceedes the range of linearity upper limit in upper machine solution, need to be with constant volume solvent by upper Within machine solution concentration is diluted to the range of linearity.
Step (1) if in the sample of the moisture content less such as sample animal livers, suitable quantity of water must be added before extraction and fully infiltrate.
In step (4), GC conditions is: chromatographic column: HP-5MS capillary chromatographic column, column length 30m, internal diameter 0.25 Mm, thickness 0.25 μm；Injector temperature 250 DEG C；Carrier gas: He, not shunt mode sample introduction, sample size: 1 μ L；Constant current mould Formula, flow velocity 1.2mL/min；Heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C with the speed of 20 DEG C per minute, so After rise 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, keep 10min；Transmission line temperature Degree: 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；Multiple-reaction monitoring scan mode MRM, monitoring parameter is:
When step (4) measures sample liquid and extraction standard working solution, if sample liquid Pesticides chromatographic peak retention time and standard In solution, corresponding pesticide retention time is consistent, and in the sample mass spectrum after background correction, selected ion all occurs, And abundance of ions is more consistent than the abundance of ions ratio with standard solution, then can determine whether sample liquid exists this pesticide；If above-mentioned two Individual condition can not meet simultaneously, then judge without this kind of pesticide.
The beneficial effects of the present invention is:
The present invention utilizes dispersive solid-phase extraction technology, establishes simplicity, quickly and can be prevented effectively from the sample of sample mesostroma interference Product pre-treating method, this pre-treating method combines GC-MS/MS, and to be applied in Cereals, animal derived food fluorine azoles bacterium aniline fixed Property confirmation and detection by quantitative, average recovery rate is 86.9%～88.1%, and average relative standard's deviation (RSD) is 6.6%～8.4%, Detection limit is less than 0.010 μ g/kg, has easy and simple to handle, quick, accurate, highly sensitive and reproducible advantage.Can meet The U.S., European Union, the Japan and other countries technology requirement to corresponding product safety detection, for ensureing our people's food safety and externally Export trade sound development provides strong technical support.
Accompanying drawing explanation
Fig. 1 is that the GC-MS/MS being added on the fluorine azoles bacterium aniline mark liquid in blank Carnis Sus domestica substrate selects chromatography of ions figure.
Fig. 2 is that the GC-MS/MS of the Carnis Sus domestica blank sample of the most fluorine-containing azoles bacterium aniline selects chromatography of ions figure.
Fig. 3 is the fluorine azoles bacterium aniline standard working curve with the Carnis Sus domestica blank sample of the most fluorine-containing azoles bacterium aniline as substrate preparation.
Detailed description of the invention
Now with following embodiment, the present invention is described, but is not to limit the scope of the present invention.
The instrument used in embodiment and reagent
T18 Basic homogenizer (IKA, Germany)；CR21G III centrifuge (Hitachi, Japan)；MS3 basic model vortex mixes Device (IKA, Germany)；TurboVap LV pattern product automatic concentration instrument (Caliper, USA)；7890N gas chromatogram-5977C Mass spectrograph (Agilent, USA)；Enhancement mode lipid is removed product (Enhanced Matrix Removal, EMR) and is purchased from the U.S. Anjelen Sci. & Tech. Inc.
Reagent
Acetonitrile, acetone, normal hexane (HPLC level, Merke, Germany)；Anhydrous magnesium sulfate, sodium chloride are analytical pure, are purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
Standard substance: purity 99.5%, purchased from Dr.Ehrenstorfer company of Germany.
Embodiment 1: the detection of fluorine azoles bacterium aniline residue amount in Carnis Sus domestica
(1) sample pre-treatments
Extract
Weigh through the abundant 5g Carnis Sus domestica sample mixed in 50mL centrifuge tube, after adding 10mL water recovery 30min, accurately add 20mL Acetonitrile solution, mechanical shaking extraction 20min, supersound extraction 5min, add 3g anhydrous magnesium sulfate and 2g sodium chloride, after vortex 1min, After 7000r/min is centrifuged 5min, to be clean.
Purify
Addition 4mL water is in the purification pipe removing product E MR equipped with enhancement mode lipid, and vortex makes it fully activate, and pipettes 6mL sample Extracting solution is in the EMR activated purifies pipe, and after vortex 1min, 7000r/min is centrifuged 5min, shifts whole supernatant to dress Have in the centrifuge tube of anhydrous magnesium sulfate and sodium chloride and saltout, after vortex centrifugal, pipette 1mL supernatant, after being concentrated to dryness, Dissolve constant volume with the acetone that volume ratio is 1/1/normal hexane mixed solvent, after crossing film, treat gas chromatogram tandem mass spectrum (GC-MS/MS) Detection.
(2) preparation of standard working solution
Accurately weighing 25 ± 0.1mg standard substance in 25mL volumetric flask, dissolve with acetonitrile, constant volume obtains 1000.0 μ g/mL standard reserving solutions； Pipette 1.0mL standard reserving solution to be placed in 100mL volumetric flask, obtain with the acetone that volume ratio is 1/1/normal hexane mixed solvent constant volume 10.0 μ g/mL standard intermediate liquids；The Carnis Sus domestica blank sample of the most fluorine-containing azoles bacterium aniline is processed by above-mentioned pre-treatment step, takes 8mL Blank extraction and cleaning liquid, after being concentrated to dryness, adds acetone/normal hexane mixed solvent vortex that 8mL volume ratio is 1/1 and dissolves, use This solution is finally configured to 1,2,5,10,20,50 μ g/L extraction standard working solutions.
(3) gas chromatogram tandem mass spectrometry (GC-MS/MS) measures
The standard working solution of variable concentrations gradient is injected separately into GC-MS/MS, carries out quantitatively dividing of fluorine azoles bacterium aniline content with external standard method Analysis, i.e. carries out regression analysis with the chromatographic peak area of standard working solution to its respective concentration, obtains standard working curve；Identical Under the conditions of sample extracting solution injected GC-MS/MS be measured, record the chromatographic peak area of fluorine azoles bacterium aniline, generation in sample liquid Enter standard working curve, obtain fluorine azoles bacterium aniline content in sample liquid, then obtain according to the Mass Calculation of sample representated by sample liquid Fluorine azoles bacterium aniline residue amount in 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.
Furnace box heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C with the speed of 20 DEG C per minute, then with per minute The speed of 2 DEG C rises to 220 DEG C, then rises to 280 DEG C 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.
Scan mode: multiple-reaction monitoring (SRM) scan pattern；MRM detection parameter is shown in Table 1.
Table 1: the MRM of embodiment 1 detects parameter
*For quota ion pair.
Qualitative Identification: at identical conditions, if sample liquid Pesticides chromatographic peak retention time pesticide corresponding to standard solution Retention time is consistent, and in the sample mass spectrum after background correction, selected ion all occurs, and abundance of ions Ratio is consistent with the abundance of ions ratio of standard solution, then can determine whether to exist in sample liquid this pesticide；If above-mentioned two condition can not be same Time meet, then judge without this kind of pesticide.
Linear relationship:
With the chromatographic peak area of standard working solution, its respective concentration being carried out regression analysis, obtaining standard working curve is Y=37028X+1697.9, correlation coefficient is 0.9992.
Recovery of standard addition and repeatability:
The fluorine azoles bacterium aniline standard solution of 10,20 and 200 3 concentration levels of μ g/kg is added in the Carnis Sus domestica of the most fluorine-containing azoles bacterium aniline, After pesticide adds 30min, carry out the determination of residual amount by above-mentioned process step, mensuration concentration and pesticide theory are added concentration and carries out Relatively, obtaining pesticide TIANZHU XINGNAO Capsul, each pitch-based sphere parallel assay 6 times, obtain its relative standard deviation, measurement result is shown in Table 1.As can be seen from Table 1, in 3 mark-on levels, the average recovery rate of fluorine azoles bacterium aniline is 86.9%～88.1%, flat All relative standard deviations (RSD) are 6.6%～8.4%, illustrate that the response rate of the inventive method is high, reproducible.
The response rate of table 1 fluorine azoles bacterium aniline and repeatability (n=6)
Detection limit:
The fluorine azoles bacterium aniline substrate standard working solution of variable concentrations is injected GC-MS/MS, with least concentration extraction standard solution chromatograph 3 times of signal to noise ratios at peak and the cycles of concentration (cycles of concentration of Carnis Sus domestica is 0.25 times) of sample handling processes calculate detection limit, fluorine azoles The detection of bacterium aniline is limited to 0.010 μ g/kg.
Above embodiment is only to be described the preferred embodiment of the present invention, not limits the scope of the present invention Fixed, on the premise of designing spirit without departing from the present invention, it is each that technical scheme is made by this area ordinary skill technology Plant modification and improvement, all should fall in the protection domain that claims of the present invention determines.

Claims (3)

1. the GC-MS/MS rapid assay methods of a fluorine azoles bacterium aniline residue amount, it is characterised in that described method includes following Step:
(1) extract
Weigh mixing sample in tool plug centrifuge tube in, after adding suitable quantity of water, add acetonitrile solution homogenizing extract after, add sodium chloride and Anhydrous magnesium sulfate, centrifugal after violent vortex 1min；
(2) purify
By enhancement mode lipid remove product E MR use water activation, pipette sample extracting solution in activate EMR purification pipe in, vortex After 1min, 7000r/min is centrifuged 5min, shifts whole supernatant to carrying out equipped with in the centrifuge tube of anhydrous magnesium sulfate and sodium chloride Saltout, after vortex centrifugal, pipette the supernatant of certain volume, after being concentrated to dryness, with the acetone that volume ratio is 1/1/normal hexane mixing Solvent dissolves constant volume, after crossing film, treats that gas chromatogram tandem mass spectrum (GC-MS/MS) detects；
(3) preparation of standard working solution
The same kind matrix blank sample of the most fluorine-containing azoles bacterium aniline is processed by above-mentioned steps (1), (2), obtains sample extraction clean Changing residue, add appropriate solvent and standard solution, vortex mixes, and is configured to the fluorine azoles bacterium aniline series standard work of at least 3 concentration Make liquid；
(4) measure and result calculates
The standard working solution of each Concentraton gradient in step (3) is carried out GC-MS/MS mensuration, with the chromatographic peak of standard working solution Area carries out regression analysis to its respective concentration, obtains extraction standard working curve；Step (2) will be purified under the same conditions After sample liquid inject GC-MS/MS and be measured, record the chromatographic peak area of fluorine azoles bacterium aniline in sample liquid, substitute into substrate mark Quasi-working curve, obtains fluorine azoles bacterium aniline content in sample liquid, then obtains sample according to the Mass Calculation of sample representated by sample liquid Fluorine azoles bacterium aniline residue amount in product；If fluorine azoles bacterium aniline residue amount exceedes the range of linearity upper limit in upper machine solution, constant volume solvent need to be used Within upper machine solution concentration is diluted to the range of linearity.
The GC-MS/MS rapid assay methods of a kind of fluorine azoles bacterium aniline residue amount the most according to claim 1, its feature exists In, step (1) if in the sample of sample moisture content less, suitable quantity of water must be added before extraction and fully infiltrate.
The GC-MS/MS rapid assay methods of a kind of fluorine azoles bacterium aniline residue amount the most according to claim 1, it is characterised in that step Suddenly in (4), GC-MS/MS analysis condition is: chromatographic column: HP-5 MS 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 keep 2min, rise to 200 DEG C with the speed of 20 DEG C per minute, then with The speed of 2 DEG C per minute rises to 220 DEG C, then rises to 280 DEG C with the speed of 20 DEG C per minute, keeps 10min；Transmission line temperature: 290℃；Ionization pattern: electron impact ionization (EI, 70eV)；Ion source temperature 280 DEG C；Collision gas: argon；Many reactions Monitoring scan mode MRM, monitoring parameter is:
CN201610070299.7A 2016-01-30 2016-01-30 GC-MS/MS rapid measurement method for penflufen residual amount Pending CN105717220A (en)

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CN104678024A (en) * 2015-03-12 2015-06-03 郭庆龙 ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits

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Application publication date: 20160629