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GC-MS/MS (Gas Chromatography-Mass Spectrometer/Mass Spectrometer) rapid determination method for residual amount of ametoctradin

A technology of pyraclostrobin and mesoxastrobin, which is applied in the field of determination of pesticide residues, can solve the problems of high price, limited effect and limited ability, and achieve the advantages of simple operation, high sensitivity and avoiding matrix interference Effect

Inactive Publication Date: 2016-06-22
郭庆龙
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] At this stage, there are few studies on the determination methods 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 fast, simple, 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 There are reports on GC-MS / MS detection method of oxamethazone residue in food, but so far there is no report on GC-MS / MS detection method of oxamethazone residue in food and agricultural products
In addition, it is well known that the QuEChERS pretreatment technology has become the most widely used sample pretreatment method in the analysis of pesticide residues, but the QuEChERS method is mainly suitable for low-fat high-water substrates, such as most fruits and vegetables, in the face of high-fat content The capacity of the matrix is ​​limited, and it is generally necessary to add n-hexane degreasing, frozen sample extract degreasing and other steps, but the effect is limited

Method used

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  • GC-MS/MS (Gas Chromatography-Mass Spectrometer/Mass Spectrometer) rapid determination method for residual amount of ametoctradin
  • GC-MS/MS (Gas Chromatography-Mass Spectrometer/Mass Spectrometer) rapid determination method for residual amount of ametoctradin
  • GC-MS/MS (Gas Chromatography-Mass Spectrometer/Mass Spectrometer) rapid determination method for residual amount of ametoctradin

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Example 1: Detection of the residual amount of oxamethoxazole in pork

[0048] (1) Sample pretreatment

[0049] extract

[0050] Weigh 5g of fully mixed pork sample into a 50mL centrifuge tube, add 10mL of water to resuscitate for 30min, then accurately add 20mL of acetonitrile solution, shake and extract for 20min, ultrasonically extract for 5min, add 3g of anhydrous magnesium sulfate and 2g of sodium chloride, vortex After 1min, centrifuge at 7000r / min for 5min and wait for purification.

[0051] purify

[0052] Add 4mL of water to the purification tube equipped with enhanced lipid removal product EMR, vortex to fully activate, pipette 6mL sample extract into the activated EMR purification tube, vortex for 1min, and then centrifuge at 7000r / min for 5min , transfer all the supernatant to a centrifuge tube filled with anhydrous magnesium sulfate and sodium chloride for salting out, after vortex centrifugation, pipette 1mL of the supernatant, concentrate to dryness, a...

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Abstract

The invention discloses a GC-MS / MS rapid determination method for the residual amount of oxamethanil. The method is mainly used for determining the residual amount of oxamethanil in animal-derived foods with high fat content. Acetonitrile was used to homogeneously extract the residual pyraclostrobin in the sample, and the extract was dispersed and purified by Enhanced Matrix Removal (EMR) matrix, extracted and concentrated by stripping tube, and then gas chromatography-tandem mass spectrometry (GC-MS / MS) detection, using a blank matrix solution without the pesticide to be tested to establish a corrected standard working curve, and quantified by the external standard method. The average recovery rate of this method is 91.3%-99.0%, the average relative standard deviation is 5.2%-8.6%, and the detection limit is lower than 6.74 μg / kg. , Good repeatability, accurate qualitative and quantitative advantages.

Description

[0001] The invention discloses a GC-MS / MS rapid determination method for the residual amount of oxamethanil. The method is mainly used for determining the residual amount of oxamethanil in animal-derived foods with high fat content. Acetonitrile was used to homogeneously extract the residual pyraclostrobin in the sample, and the extract was dispersed and purified by Enhanced Matrix Removal (EMR) matrix, extracted and concentrated by stripping tube, and then gas chromatography-tandem mass spectrometry (GC-MS / MS) ) detection, using a blank matrix solution that does not contain the pesticide to be tested to establish a corrected standard working curve, and quantify with the external standard method. The average recovery rate of this method is 91.3%-99.0%, the average relative standard deviation (RSD) is 5.2%-8.6%, and the detection limit is lower than 6.74 μg / kg. Strong characteristics, good repeatability, and accurate qualitative and quantitative advantages. It can meet the techn...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/062
Inventor 郭庆龙
Owner 郭庆龙
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