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Determination method for residual quantity of silthiopham in vegetables and fruits

A technology for the determination of silthiocarb and its determination method, which is applied in the qualitative and quantitative determination of the content of silthiocarb residues in vegetables and fruits by gas chromatography tandem mass spectrometry, and the field of determination of silthiocarb residues, which can solve the problem of high price and relatively high cost. Long system and other problems, easy to operate, avoid matrix interference, and good repeatability

Inactive Publication Date: 2016-06-29
郭庆龙
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  • Abstract
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Problems solved by technology

[0007] At this stage, there are few studies on the determination methods of silthiocarb residues, and the detection methods reported are mainly the detection methods of silthiocarb 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 silthiocarb residues in vegetables and fruits. Using 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 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 silithiocarb residues in vegetables and fruits, so the establishment of simple, fast, accurate, durable, accurate qualitative and quantitative analysis of GC-MS / MS for fluoxetin residues in vegetables and fruits The detection method is of great significance

Method used

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  • Determination method for residual quantity of silthiopham in vegetables and fruits
  • Determination method for residual quantity of silthiopham in vegetables and fruits
  • Determination method for residual quantity of silthiopham in vegetables and fruits

Examples

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Embodiment 1

[0032] Embodiment 1: detection of silthiocarb residues in apples

[0033] (1) Sample pretreatment Weigh 10.0 g of fully 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 then 7000r / centrifuge for 5min. 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.

[0034] (2) Preparation of standard working solution Accurately weigh 25±0.1mg standard product in a 25mL volumetric fl...

Embodiment 2

[0061] Example 2: Detection of Silthiocarb Residues in Cucumber

[0062] (1) Sample pretreatment 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 , after vortexing for 1min, 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.

[0063] (2) Preparation of standard working solution

[0064] Dilute the 1000 μg / mL stan...

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Abstract

The invention discloses a determination method for the residual quantity of silthiopham in vegetables and fruits. The determination method comprises the steps that residual silthiopham in a sample is homogeneously extracted with acetonitrile or an acetonitrile solution containing 1% of acetic acid; matrix dispersion and purification are performed on an extracting solution through primary secondary amine (PSA) and octadecylsilyl (C18), and then detection is performed through gas chromatography-tandem mass spectrometry(GC-MS / MS); a corrected standard work curve is built by adopting a blank substrate solution which does not contain a pesticide to be determined, and quantifying is performed through an external standard method. According to the method, the average recovery rate is 83.0%-90.8%, the average relative standard deviation (RSD) is 5.1%-7.5%, the detection limit is lower than 0.013 milligram per kilogram, the advantages of being easy and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitative and quantitative property are achieved, the technical requirements of the states such as America, European Union and Japan for safety detection on corresponding products can be met, and powerful technical support is supplied for ensuring the food safety of people in China and healthy development of foreign export trade.

Description

technical field [0001] The invention relates to a method for determining the residual amount of silthiocarb in vegetables and fruits, more specifically, it is a method for qualitatively and quantitatively determining the residual amount of silthiocarb in vegetables and fruits by gas chromatography-tandem mass spectrometry (GC-MS / MS) The method belongs to the technical field of determination of pesticide residues. Background technique [0002] Silthiofam (common name: Silthiofam, test code: Mon65500, trade name: Latitude, other names: Silthiopham) is an amide fungicide developed by Monsanto. It is mainly used as seed treatment to control take-all disease on grains. Chemical name: N-allyl-4,5-dimethyl-2-(trimethylsilyl)thiophene-3-carboxamide, English name: N-allyl-4,5-dimethyl-2-(trimethylsilyl )thiophene-3-carboxamide, CAS accession number: 175217-20-6, chemical structural formula is: [0003] [0004] Appearance is white crystalline powder; melting point: 86.1~88.3°C;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N27/62
CPCG01N27/62G01N30/02G01N30/06G01N2030/025
Inventor 郭庆龙
Owner 郭庆龙
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