CN106324133A - Solid phase extraction-gas chromatography-tandem mass spectrum detection method for amide fungicides in wine - Google Patents
Solid phase extraction-gas chromatography-tandem mass spectrum detection method for amide fungicides in wine Download PDFInfo
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- CN106324133A CN106324133A CN201610674093.5A CN201610674093A CN106324133A CN 106324133 A CN106324133 A CN 106324133A CN 201610674093 A CN201610674093 A CN 201610674093A CN 106324133 A CN106324133 A CN 106324133A
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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
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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
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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
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- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a solid phase extraction-gas chromatography-tandem mass spectrum detection method for amide fungicides in wine. The method can detect four types amide fungicides in a sample wine at the same time, including mandipropamid, thiazole fluopicolide, silthiopham, and fluopicolide. The solid phase extraction-gas chromatography-tandem mass spectrum detection method includes the following steps: diluting the sample wine with ultra pure water to obtain the liquid to be detected, purifying the liquid to be detected with HLB solid phase extraction column, and separating the liquid to be detected with C18 reversed-phase column, performing the qualitative analysis on a target analyte in the multiple reaction monitoring mode, based on the comparison between retention time and ion pair information, and quantifying the target analyte with an isotope internal standard method. The method has fast analysis speed, high sensitivity, good reproducibility and good accuracy, and is a new detection method for the evaluation of the quality of the sample wine.
Description
Technical field
The invention belongs to field of food detection, relate to Solid-Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), tool
Body refers to 4 kinds of acid amide fungicides such as mandipropamid, Guardian, Silthiopham, fluopicolide in a kind of wine
Detection method, is particularly suited for wine.
Background technology
Along with raising and the enhancing of health perception of people's living standard, this collection trophism of wine, functional and
Cultural taste is increasingly liked by people in the special beverage of one.Zhejiang is more flourishing as China's southeastern coast economy
Province, in recent years wine consumption figure rapid development, particularly import wine.Port, the Zhejiang import wine volume of trade is always
Occupy leading position of the same trade, the whole nation.2015, port, Zhejiang import wine 3.11 ten thousand tons altogether, increase by 10.2% than last year, value of goods
1.2 hundred million dollars, market transaction volume 3,500,000,000 yuan, import volume ranking is only second to the ports such as Shanghai, Shenzhen and Guangzhou, Tianjin.Wine disappears
The fiery degree in expense market has some idea of.
But, whether import or domestic wine, Fructus Vitis viniferae as its topmost raw materials for production in field management
Cheng Zhong, for preventing disease from occurring, it will usually spray a certain amount of pesticide, some pesticide is difficult in Production of Wine sweat
Remove and decompose, can remain in wine to some extent, bring potential threat to drinking person health.2013, U.S.'s ring
In " the dirtiest fruit and vegerable " blacklist that border working group (EWG) issues, Fructus Vitis viniferae ranks the 3rd, altogether 15 kinds of residue of pesticide compositions of detection,
And in terms of the pesticide variety contained, Fructus Vitis viniferae then ranks first, altogether contain 64 kinds of different chemical substances.Therefore, wine
In Pesticide Residue should not be underestimated.
At present, amides pesticide maximum residue limit in food has been done strict regulations, such as European Union by some country
Rules and regulations: the maximum residue limit of mandipropamid (Mandipropamid) is 2.0 mg/kg in Fructus Vitis viniferae, fluopicolide
(Fluopicolide) maximum residue limit is 2.0 mg/kg, and the maximum residue limit of Silthiopham (Silthiofam) is the lowest
To 0.01 mg/kg.These regulations, while protection consumer health's interests, are also important TBT (Technical Barriers to Trade) measures.
Therefore, set up and accurately and reliably measure mandipropamid, Guardian, Silthiopham, fluorine pyridine acyl bacterium in wine
The content of 4 kinds of acid amide fungicides such as amine is extremely important.
At present, conventional analysis method can be divided into qualitative analysis, quantitative analysis and qualitative and quantitative analysis technology.Quantitative analysis
General employing chromatographic technique and hydrolysis and condensation, chromatographic technique has the method such as gas chromatogram and liquid chromatograph, chromatograph matter
Spectrum multiple techniques has the method such as liquid chromatograph mass spectrography and gas chromatography-mass spectrography；Qualitative and quantitative analysis then to have two concurrently
The technology of kind is integrated, and testing result to provide structural information and the quantity information of object simultaneously, non-by force according to EU Committee
System performs the regulation of bill 2002/657/EC, and the method that forbidden drugs carries out confirmation detection must be able to provide configuration aspects
Information, and to reach 4 confirmation points of this bill regulation.
At present, owing to can follow without relevant criterion or document both at home and abroad, therefore, it is necessary to the mandipropamid in wine
The detection method of 4 kinds of acid amide fungicides such as amine, Guardian, Silthiopham, fluopicolide is studied, thus to Fructus Vitis viniferae
In wine, acid amide fungicides is monitored, and when exporting to the areas such as European Union for domestic Wine Enterprises simultaneously, can provide and meet Europe
The detection data of the regulation of committee of alliance optional execution bill 2002/657/EC.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides the liquid phase color of acid amide fungicides in a kind of wine
Spectrum-tandem mass spectrum detection method, the method combines Solid-Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry, it is possible to alkynes double in wine
4 kinds of acid amide fungicides such as acyl bacterium amine, Guardian, Silthiopham, fluopicolide are measured simultaneously, and the method has standard
Really, quick, highly sensitive advantage, the quickly detection for wine provides reliable detection method support.
To achieve these goals, the technical solution used in the present invention is: in a kind of wine, acid amide fungicides consolidates
Extraction-liquid chromatography-tandem mass mutually, it is characterised in that comprise the following steps:
(1) preparation of testing sample: weigh 4.7-5.3g wine sample, adds ultra-pure water in wine sample, after mixing
To liquid to be checked；
(2) purification of liquid to be checked: fixing phase extraction column is carried out pretreatment, the liquid to be checked step () prepared fixes phase
Extraction column, removes impurity through water and methanol/water solution drip washing, then fixes the mandipropamid on phase extraction column with eluting solvent eluting
Amine, Guardian, Silthiopham, fluopicolide obtain eluent, after eluent enrichment method, dilute also with methanol solvate
Testing sample solution is obtained after 0.22 μm filtering with microporous membrane；
(3) configuration of standard solution: prepare mandipropamid, Guardian, Silthiopham, fluopicolide solution rank respectively
Hybrid standard working solution 1.0 ng/mL, 2.0 ng/mL, 5.0 ng/mL, 10.0 ng/mL, 20.0 ng/mL of ladder concentration,
Internal standard substance Guardian-D5 concentration is 10.0 ng/mL,
(4) detection of testing sample solution: by the testing sample solution in step (two) and hybrid standard working solution in liquid phase
Difference sample introduction on chromatograph-tandem mass spectrometer, it is thus achieved that with mandipropamid, Guardian, Silthiopham, fluorine pyridine acyl in standard solution
Bacterium amine, the concentration of Guardian-D5 are abscissa, then with mandipropamid, Guardian, silicon thiophene in hybrid standard working solution
Bacterium amine, fluopicolide, the working curve that peak area is vertical coordinate of Guardian-D5, also acquisition may determine that parent ion
Mandipropamid, Guardian, Silthiopham, fluopicolide, the first mass spectrometric figure of Guardian-D5, determine parent ion
After, use daughter ion scanning to obtain second order ms figure, from second order ms figure, then choose quota ion and qualitative ion, then
With working curve, quota ion carried out quantitative Analysis, inner mark method ration (internal standard substance is Guardian-D5), it is thus achieved that testing sample
The concentration of mandipropamid, Guardian, Silthiopham, fluopicolide in solution.
Further, the fixing phase extraction column in described step (two) is Waters Oasis HLB SPE post, and passes through
Methanol, water carry out activation processing to SPE post.
Further, the drip washing solvent in described step (two) is water and methanol-water mixed solution that volume ratio is 1/3, washes
Desolventizing is methanol.
Further, in described step (three), the detection parameter of liquid chromatography-tandem mass spectrometry instrument is:
Chromatographic column: Agilent ZORBAX Eclipse Plus C18Reversed-phase column；
Flow velocity: 0.25 mL/min；
Flowing phase: A is 0.15% aqueous formic acid；B is acetonitrile；
Sample size: 5 μ L；
Chromatogram column temperature: 30 C；
Electric spray ion source: cation scans, and voltage is 5000V；
Ion source temperature: 450 C；
Atomization gas pressure: 50 psi；
Secondary air speed: 40 psi；
Gas curtain atmospheric pressure: 20 psi；
Collision atmospheric pressure: 20 psi.
Using such scheme, wine samples is diluted by the present invention by adding ultra-pure water, and to dilute by ultra-pure water
Releasing the liquid to be checked obtained and carry out purified treatment, this purified treatment includes the process of purification and enrichment.First step purification: first by be checked
Liquid passes through solid phase extraction column, sequentially passes through through water and methanol/water solution drip washing, methanol-eluted fractions；Second step is enriched with: by the first step
The liquid nitrogen gas to be checked of middle purification concentrates near dry, be subsequently adding methanol solution dissolve, through 0.22 μm filtering with microporous membrane, be purified
Liquid to be checked.Detecting instrument then will not be polluted by the liquid to be checked after this purification.In the present invention, the SPE post of Solid-Phase Extraction is
Waters Oasis HLB SPE post, owing to the polarity size of 4 kinds of acid amide fungicides He other impurity there are differences, in solid phase
On extraction column, absorption produces and retains difference, then by preferred drip washing condition and elution requirement, reaches purification enrichment antibacterial
Purpose.
Secondly, the present invention is for the mandipropamid in wine, Guardian, Silthiopham, fluopicolide etc. 4 kinds
The qualitative and quantitative detection analysis of acid amide fungicides composition is to be analyzed by liquid chromatography-tandem mass spectrometry instrument (LC-MS/MS).First
Configure one group of step-like standard working solution, then by standard working solution and liquid to be checked on liquid chromatography-tandem mass spectrometry instrument
Sample introduction respectively.The chromatographic peak retention time occurred in liquid to be checked is consistent with standard working solution, it is allowed to deviation is less than ± 2.5 %,
The relative abundance of the standard working solution that the relative abundance of the mass spectrometry ion corresponding to this chromatographic peak is suitable with concentration is consistent,
And relative abundance deviation is less than regulation, then can determine that in this liquid to be checked containing acid amide fungicides.
Finally, this method uses Internal standard to carry out quantitatively, more accurate to quantitative result.
The invention will be further described below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Accompanying drawing 1 is the Guardian chemical structural formula in the specific embodiment of the invention；
Accompanying drawing 2 is the mandipropamid chemical structural formula in the specific embodiment of the invention；
Accompanying drawing 3 is the fluopicolide chemical structural formula in the specific embodiment of the invention；
Accompanying drawing 4 is the Silthiopham chemical structural formula in the specific embodiment of the invention；
Accompanying drawing 5 is the Guardian-D5 chemical structural formula in the specific embodiment of the invention；
Accompanying drawing 6 is Guardian antibacterial standard solution (1.0 ng/mL) MRM chromatogram in the specific embodiment of the invention；
Accompanying drawing 7 is mandipropamid antibacterial standard solution (1.0 ng/mL) MRM chromatogram in the specific embodiment of the invention；
Accompanying drawing 8 is fluopicolide antibacterial standard solution (1.0 ng/mL) MRM chromatogram in the specific embodiment of the invention；
Accompanying drawing 9 is Silthiopham antibacterial standard solution (1.0 ng/mL) MRM chromatogram in the specific embodiment of the invention；
Accompanying drawing 10 is Guardian-D5 antibacterial standard solution (1.0 ng/mL) MRM chromatogram in the specific embodiment of the invention
Accompanying drawing 11 is Guardian antibacterial scanning second order ms figure in the specific embodiment of the invention；
Accompanying drawing 12 is mandipropamid antibacterial scanning second order ms figure in the specific embodiment of the invention；
Accompanying drawing 13 is fluopicolide antibacterial scanning second order ms figure in the specific embodiment of the invention；
Accompanying drawing 14 is Silthiopham antibacterial scanning second order ms figure in the specific embodiment of the invention；
Accompanying drawing 15 is Guardian-D5 antibacterial scanning second order ms figure in the specific embodiment of the invention；
Accompanying drawing 16 is Guardian standard working curve in the specific embodiment of the invention；
Accompanying drawing 17 is mandipropamid standard working curve in the specific embodiment of the invention；
Accompanying drawing 18 is fluopicolide standard working curve in the specific embodiment of the invention；
Accompanying drawing 19 is Silthiopham standard working curve in the specific embodiment of the invention.
Detailed description of the invention
The specific embodiment of the present invention is the liquid chromatography-tandem matter of acid amide fungicides in wine as shown in figures 1-19
Spectrum detection method, it comprises the following steps:
The preparation of testing sample: weigh wine samples 5.0g, adds 3 mL ultra-pure waters and is uniformly mixed so as to obtain liquid to be checked；
Solid phase extraction: take HLB SPE post, activates SPE post with first alcohol and water successively, takes whole liquid to be checked to SPE post, then depends on
Secondary with 4～6mL water with 4～6mL methanol/water mixed solutions (v/v, 1/3) drip washing SPE post, SPE post vacuum is drained, with 6～
The methanol of 8mL carries out eluting to SPE post, obtains eluent, after being concentrated by eluent, after crossing microporous filter membrane with 2 mL methanol dilution
Obtain testing sample solution；
The configuration of standard solution: take mandipropamid, Guardian, Silthiopham, fluopicolide, Guardian-D5 standard
Product, are configured to the list mark storing solution that mass concentration is 400 mg/L respectively with methanol, when being measured using, with on methanol dilution
State standard reserving solution, mandipropamid, Guardian, Silthiopham, fluopicolide are configured to respectively 1.0ng/mL, 2.0
The hybrid standard working solution of ng/mL, 5.0 ng/mL, 10.0 ng/mL, 20.0 ng/mL, internal standard substance Guardian-D5 concentration
It is 10.0 ng/mL；
The detection of testing sample: by the testing sample solution in step (two) (three) and standard working solution at liquid chromatograph-string
Difference sample introduction on connection mass spectrograph, it is thus achieved that with mandipropamid, Guardian, Silthiopham, fluopicolide etc. 4 in standard solution
The concentration planting acid amide fungicides is abscissa, then with mandipropamid, Guardian, Silthiopham, fluorine pyridine in standard solution
4 kinds of acid amide fungicides such as acyl bacterium amine the working curve that peak area is vertical coordinate, result shows, 4 kinds of acid amide fungicides
There is in the range of 1.0-20.0 ng/mL good linear relationship, R2>=0.99, it is that method is quantitative with 10 times of signal to noise ratios (S/N)
Limit i.e. LOQ, adds test through sample and determines that the quantitative limit of 4 kinds of acid amide fungicides is 0.5 ng/g.Also acquisition can be true
Determine the first mass spectrometric of 4 kinds of acid amide fungicides such as the mandipropamid of parent ion, Guardian, Silthiopham, fluopicolide
Figure, after determining parent ion, use daughter ion scanning obtain second order ms figure, then choose from second order ms figure quota ion and
Qualitative ion, then carries out quantitative Analysis with working curve to quota ion, inner mark method ration (internal standard substance be Guardian-
D5), it is thus achieved that 4 kinds of amide-type sterilizations such as mandipropamid, Guardian, Silthiopham, fluopicolide in testing sample solution
The concentration of agent.
1-4 kind of acid amide fungicides LC-MS/MS testing conditions of table
*MS/MS quota ion pair
Table 2-4 kinds of linear equation of acid amide fungicides, correlation coefficient, quantitative limit
-4 kinds of acid amide fungicides TIANZHU XINGNAO Capsul of table, precision (n=6)
The present invention is not limited to above-mentioned detailed description of the invention, and persons skilled in the art, can according to present disclosure
To use other multiple detailed description of the invention to implement the present invention, or the design structure of every employing present invention and thinking, do
Simple change or change, both fall within protection scope of the present invention.
Claims (4)
1. Solid-Phase Extraction-the liquid chromatography-tandem mass of acid amide fungicides in a wine, it is characterised in that
Comprise the following steps:
The preparation of testing sample: weigh 4.7-5.3g wine sample, adds ultra-pure water, is treated after mixing in wine sample
Inspection liquid；
The purification of liquid to be checked: fixing phase extraction column is carried out pretreatment, the liquid to be checked step () prepared is fixed and extracts mutually
Post, removes impurity through water and methanol/water solution drip washing, then with eluting solvent eluting fix the mandipropamid on phase extraction column,
Guardian, Silthiopham, fluopicolide obtain eluent, after eluent enrichment method, with methanol solvate dilution warp
Testing sample solution is obtained after 0.22 μm filtering with microporous membrane；
The configuration of standard solution: prepare mandipropamid, Guardian, Silthiopham, fluopicolide solution ladder respectively dense
Hybrid standard working solution 1.0 ng/mL of degree, 2.0 ng/mL, 5.0 ng/mL, 10.0 ng/mL, 20.0 ng/mL, internal standard
Thing Guardian-D5 concentration is 10.0 ng/mL,
The detection of testing sample solution: by the testing sample solution in step (two) and hybrid standard working solution at liquid phase color
Difference sample introduction on spectrum-tandem mass spectrometer, it is thus achieved that with mandipropamid, Guardian, Silthiopham, fluorine pyridine acyl bacterium in standard solution
Amine, the concentration of Guardian-D5 are abscissa, then with mandipropamid, Guardian, silicon thiophene bacterium in hybrid standard working solution
Amine, fluopicolide, the working curve that peak area is vertical coordinate of Guardian-D5, also have acquisition to may determine that parent ion
Mandipropamid, Guardian, Silthiopham, fluopicolide, the first mass spectrometric figure of Guardian-D5, after determining parent ion,
Use daughter ion scanning to obtain second order ms figure, from second order ms figure, then choose quota ion and qualitative ion, then use
Working curve carries out quantitative Analysis, inner mark method ration (internal standard substance is Guardian-D5), it is thus achieved that testing sample is molten to quota ion
The concentration of mandipropamid, Guardian, Silthiopham, fluopicolide in liquid.
Solid-Phase Extraction-the liquid chromatography-tandem mass spectrometry of acid amide fungicides in a kind of wine the most according to claim 2
Detection method, it is characterised in that: the fixing phase extraction column in described step (two) is Waters Oasis HLB SPE post, and leads to
Cross methanol, water carries out activation processing to SPE post.
Solid-Phase Extraction-the liquid chromatography-tandem mass spectrometry of acid amide fungicides in a kind of wine the most according to claim 2
Detection method, it is characterised in that: the drip washing solvent in described step (two) be water and the mixing of methanol-water that volume ratio is 1/3 molten
Liquid, eluting solvent is methanol.
Solid-Phase Extraction-the liquid chromatography-tandem mass spectrometry of acid amide fungicides in a kind of wine the most according to claim 2
Detection method, it is characterised in that: in described step (three), the detection parameter of liquid chromatography-tandem mass spectrometry instrument is:
Chromatographic column: Agilent ZORBAX Eclipse Plus C18Reversed-phase column；
Flow velocity: 0.25 mL/min；
Flowing phase: A is 0.15% aqueous formic acid；B is acetonitrile；
Sample size: 5 μ L；
Chromatogram column temperature: 30 C；
Electric spray ion source: cation scans, and voltage is 5000V；
Ion source temperature: 450 C；
Atomization gas pressure: 50 psi；
Secondary air speed: 40 psi；
Gas curtain atmospheric pressure: 20 psi；
Collision atmospheric pressure: 20 psi.
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Cited By (1)
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