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

A technology of penthiopyram, fruits and vegetables, applied in the field of determination of pesticide residues, can solve the problems of relatively long system consumption and high price, and achieve the effects of avoiding matrix interference, simple operation and high sensitivity

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 methods of penthiopyram residues, and the detection methods reported are mainly the detection methods of penthiopyram residues in vegetables and fruits. These detection methods all use liquid chromatography tandem mass spectrometry (LC-MS / MS) is a detection method for the determination of penthiopyram residues in vegetables and fruits. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of fast, simple, and high sensitivity. However, due to its high price, many testing institutions and enterprises Or the scientific research institute has not configured this instrument or the number of equipment is small. 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 and mobile phases and takes a long time. The time to balance the system restricts the application of LC-MS / MS to some 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 GC-MS / MS detection method for penthiopyram residues, so the establishment of simple, fast, accurate, durable, accurate qualitative and quantitative analysis of GC-MS / MS for fluoxetyram residues in vegetables and fruits The detection method is of great significance

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

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Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Detection of Penthiopyrad 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 18and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 1mL 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 produ...

Embodiment 2

[0067] Example 2: Detection of Penthiopyrad Residues in Cucumber

[0068] (1) Sample pretreatment

[0069] 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 in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 1mL 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 well, then transfer it to an injection bottle for GC-MS / MS determination.

[0070] (2) Preparation of standard working solution

[0071] Dilute the 1000 μg / mL st...

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Abstract

The invention discloses a method for determining penthiopyrad 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 penthiopyrad 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 92.2 percent to 101.3 percent; the average RSD (relative standard deviation) is 3.9 percent to 7.3 percent; the detection limit is lower than 0.26mug / 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 present invention relates to a GC-MS / MS method for determining the residues of Penthiopyrad in fruits and vegetables, more specifically, using gas chromatography-tandem mass spectrometry (GC-MS / MS) to qualitatively and quantitatively determine the residues of Penthiopyrad in vegetables and fruits The invention discloses a method for amine content, which belongs to the technical field of determination of pesticide residues. Background technique [0002] Penthiopyrad (Penthiopyrad) is a novel amide fungicide developed by Mitsui Chemicals, Japan. Its English common name is penthiopyrad, its test code is MTF-753, and its trade name is Afetofluapro. CAS registration number: 183675-82-3, chemical name is (RS)-N-[2-(1,3-dimethylbutyl)-3-thienyl]-methyl-3-(trifluoromethyl )-1H-pyrazole-4-carboxamide, the chemical structural formula is: [0003] [0004] Penthiopyrad has a different bactericidal spectrum from the existing carboxamide fungicides. In add...

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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