Method for detecting imidaclothiz content in livestock and poultry meat

A technology for chlorothiline and livestock and poultry meat is applied in the field of detection of chlorothiline drug residues, which can solve the problems of unsuitable chlorothiline residue detection, low detection limit, inability to meet trace-level drug residues, and the like, and achieves linearity. The effect of good relationships, fast analysis, and easy operation

Inactive Publication Date: 2019-05-10
北京市营养源研究所有限公司
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Problems solved by technology

Since the pretreatment method of plant-derived samples is not suitable for fresh meat samples containing high protein and fat, the above method is not suitable for the detection of chlorothialine residues in livestock and poultry meat
In addition, the minimum detection limit of the above method: liquid chromatography 3.43 × 10 -2 mg / kg, 0.05 mg / kg by GC-MS, 2.5 mg / kg by colloidal gold immunochromatography, and 0.8 mg / kg by capillary electrophoresis, which cannot meet the needs of trace drug residues

Method used

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  • Method for detecting imidaclothiz content in livestock and poultry meat
  • Method for detecting imidaclothiz content in livestock and poultry meat
  • Method for detecting imidaclothiz content in livestock and poultry meat

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The detection of chlorothialine in embodiment 1 pork

[0075] Sample to be tested in this embodiment: commercially available pork.

[0076] Using liquid chromatography tandem mass spectrometry to detect the content of chlorothialine in livestock and poultry meat, the method is as follows:

[0077] 1) Sample pretreatment

[0078] After homogenizing the sample to be tested with a homogenizer, accurately weigh 2.00g of the sample (accurate to 0.01g) into a 50mL centrifuge tube, add 10mL of acetonitrile, 0.1mL of formic acid, 1.00g of sodium chloride, and 4.00g of anhydrous sodium sulfate . Tighten the cap of the centrifuge tube and extract by vortexing for 1 min, then centrifuge at 5000 r / min for 5 min at 10°C.

[0079] Transfer the upper organic phase to a 25 mL centrifuge tube containing 50 mg PSA sorbent and 150 mg C18 sorbent. After tightening the cap of the centrifuge tube, vortex for 1 min, and centrifuge at 5000 r / min for 5 min at 10°C.

[0080] The supernatant...

Embodiment 2

[0101] The detection of chlorothialine in embodiment 2 beef

[0102]The sample to be tested in this example: commercially available beef.

[0103] The detection method is the same as in Example 1.

[0104] According to the negative beef matrix sample prepared in this example, the corresponding peak areas were measured as 4977, 17526, 46355, 103982, 213536, respectively, and the corresponding concentrations calculated according to the amount of chlorothiline added were 1.0ng / mL, 2.0ng / mL For standard series of mL, 5.0ng / mL, 10ng / mL and 20ng / mL, the peak area corresponds to the concentration, and the least squares method is used to calculate the calibration curve of chlorothiline matrix addition as Y=10970X-6094.4R 2 =0.9997. where Y is the response value and X is the concentration.

[0105] The mass chromatogram of chlorothiline in beef matrix is ​​shown in image 3 .

[0106] The test sample solution obtained after the pretreatment of the sample to be tested was injected ...

Embodiment 3

[0108] The detection of chlorothiline in embodiment 3 mutton

[0109] The sample to be tested in this example: commercially available mutton.

[0110] The detection method is the same as in Example 1.

[0111] According to the negative mutton matrix sample prepared in this example, the corresponding peak areas were measured as 5298, 19687, 56540, 124921, and 248625 respectively. mL, 5.0ng / mL, 10ng / mL, 20ng / mL standard series, the peak area corresponds to the concentration, and the least squares method is used to calculate the calibration curve of chlorothiline matrix addition as Y=12813X-6366.1R 2 =0.9996. where Y is the response value and X is the concentration.

[0112] The mass chromatogram of chlorothiline in mutton matrix is ​​shown in Figure 4 .

[0113] result calculation

[0114] After pretreatment of the sample to be tested, the obtained sample solution to be tested was injected into the liquid chromatography-mass spectrometer, and the corresponding peak area w...

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Abstract

The invention relates to a method for detecting the imidaclothiz content in livestock and poultry meat, and belongs to the technical field of food detection. According to the method in the invention,a to-be-detected sample pre-treatment method and a liquid chromatogram and mass spectrometry condition are optimized; and the disadvantage that the imidaclothiz drug reside in the livestock and poultry meat cannot be measured by the existing method is solved. According to the method in the invention, the linear relationship in a 10-400 ng / mL range is good; the detection limit is 5.0 mug / kg; the method recovery rate in different livestock and poultry meat substrates is 91.41-93.51%; and the relative standard deviation is 2.4-3.2%. The method disclosed by the invention has the characteristics ofbeing simple and convenient to operate, rapid in analysis speed, high in sensitivity and good in reproducibility, and has great significance for quantitative detection of the imidaclothiz drug residein the livestock and poultry meat in the field of food detection.

Description

technical field [0001] The invention relates to a detection method for chlorothialine drug residues in livestock and poultry meat, and belongs to the technical field of food detection. Background technique [0002] Chlorthialine is a neonicotinoid insecticide, which is a new type of pesticide after organophosphorus, organochlorine, carbamate and pyrethroid insecticides. Chlorthialine has a wide insecticidal spectrum and has a good control effect on Coleoptera, Diptera and Lepidoptera pests, especially has relatively high toxicity to leafhoppers, rice planthoppers, thrips, and rice borers. And because of its low price, more and more planters use chlorothialine to replace the original pesticides to prevent and control insect pests. If the operation of pesticide application is not scientific, it will often cause pesticides in crops to exceed the standard. As the downstream of the food chain, livestock and poultry eat corn, soybean meal, bran, wheat bran and other crop product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14G01N30/34G01N30/86
Inventor 周大卫崔亚娟鲁绯李东
Owner 北京市营养源研究所有限公司
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