Method for determining ametoctradin residue in fruits and vegetables through GC-MS/MS (gas chromatography-tandem mass spectrometry)

A technology based on pyraclostrobin and pyraclostrobin, which is applied in the field of pyraclostrobin residues, can solve the problems of long system, few methods for measuring the amount of pyrazastrobin residues, high price, etc., and achieve repeatability Good performance, protection of people's food safety, and easy operation

Inactive Publication Date: 2016-05-04
郭庆龙
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Problems solved by technology

[0006] At this stage, there are few studies on the determination of oxamethazone residues. The detection methods reported are mainly the detection methods of oxamethazone residues in vegetables and fruits. These detection methods are all based on liquid chromatography tandem mass spectrometry (LC- MS / MS) is a detection method for the determination of oxamethazone residues in vegetables and fruits. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, and high sensitivity. However, due to its high price, many detection methods Institutions, enterprises or scientific research institutes are not equipped with this instrument or have a small number of units. Since different compounds are detected by LC-MS / MS, different mobile phases or chromatographic columns need to be used, which requires constant replacement of chromatographic columns, mobile phases and It takes a long time to balance the system, which restricts the application of LC-MS / MS to a certain extent
The use of gas chromatography-tandem mass spectrometry (GC-MS / MS) to analyze pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, high sensitivity, and strong selectivity. It can achieve multi-residue analysis of hundreds of pesticides, but so far no food and agricultural products The report of the GC-MS / MS detection method for the residues of oxamethyzil in vegetables and fruits, so the establishment of a simple, fast, accurate, durable, accurate qualitative and quantitative analysis of GC-MS / MS detection method is of great significance

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  • Method for determining ametoctradin residue in fruits and vegetables through GC-MS/MS (gas chromatography-tandem mass spectrometry)
  • Method for determining ametoctradin residue in fruits and vegetables through GC-MS/MS (gas chromatography-tandem mass spectrometry)
  • Method for determining ametoctradin residue in fruits and vegetables through GC-MS/MS (gas chromatography-tandem mass spectrometry)

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Detection of oxamethoxam residues in apples

[0035] (1) Sample pretreatment

[0036] Weigh 10.0 g of well-mixed apples into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, homogeneously extract for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium chloride, vortex for 1 min, and centrifuge at 7000 r / min for 5 min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA centrifuge tube, vortex 1min, 5000r / min centrifugation 5min. Take 4mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly, pass through the membrane, and transfer it to the sample bottle for GC- MS / MS determination.

[0037] (2) Preparation of standard working solution

[0038]Accurately weigh 25±0.1mg of the standard product in a 25mL volu...

Embodiment 2

[0066] Example 2: Detection of oxamethazone residues in cucumber

[0067] (1) Sample pretreatment

[0068] Weigh 10.0 g of well-mixed cucumber into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate, 2 g of sodium acetate and 2 mL of water, vortex for 1 min, Centrifuge at 7000r / min for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA centrifuge tube, vortex 1min, 5000r / min centrifugation 5min. Take 4mL of the supernatant in a nitrogen blowpipe and dry it with nitrogen at 40°C. Add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue. / MS determination.

[0069] (2) Preparation of standard working solution

[0070] Dilute the 1000 μg / mL standard intermediate solution with acetone / n-hexane mixed solvent with a volume ratio...

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Abstract

The invention discloses a method for determining ametoctradin residue in fruits and vegetables through GC-MS/MS (gas chromatography-tandem mass spectrometry). Acetonitrile or an acetonitrile solution containing one-percent acetic acid is used for performing homogeneous extraction of residual ametoctradin in samples; after an extracting solution is subjected to PSA(primary secondary amine)/C<18> (octadecylsilyl) matrix dispersed purification, GC-MS/MS detection is performed; a corrected standard work curve is built by using a blank matrix solution not containing pesticide to be detected; an external reference method is used for quantification. The method has the advantages that the average recovery rate is 84.3 percent to 90.6 percent; the average RSD (relative standard deviation) is 5.0 percent to 8.0 percent; the detection limit is lower than 3.40mug/kg; the operation is simple, convenient and fast; the sensitivity is high; the repeatability is good; the qualitative and quantitative analysis is accurate. The technical requirements of countries such as America, European Union and Japan on corresponding product safety detection can be met; powerful technical support is provided for guaranteeing the food safety of Chinese people and healthy development of export abroad trade.

Description

technical field [0001] The invention relates to a GC-MS / MS method for determining the residues of oxamethoxam in fruits and vegetables, more specifically, the qualitative and quantitative determination of benzopyridine residues in vegetables and fruits by gas chromatography tandem mass spectrometry (GC-MS / MS) The invention discloses a method for azoxystrobin content, belonging to the technical field of pesticide residue determination. Background technique [0002] Ametoctradin (Ametoctradin) is a new type of fungicide developed by BASF. a] pyrimidine-7-amine, the chemical formula is C15H25N5, and the structural formula is: [0003] [0004] Ametoctradin belongs to the class of s-triazolopyrimidines. It functions as a mitochondrial respiration inhibitor and can prevent and control oomycete fungal diseases, such as downy mildew and various diseases. Ametoctradin was first approved or approved in the European Union and South America in 2010, and has been registered in many...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06G01N2030/025G01N2030/062G01N2030/8809
Inventor 郭庆龙
Owner 郭庆龙
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