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Sample pretreatment and detection method for determining content of pesticide residues in cow milk

A technology for sample pretreatment and pesticide residues, applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as affecting the accuracy of test results, retention of unfavorable compounds, and loss of target substances, reducing impact, improving recovery, Results with high accuracy

Inactive Publication Date: 2021-10-01
JUNLEBAO DAIRY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are few methods for the determination of pesticide residues in milk. GB / T 23210-2008 and GB / T23211-2008 respectively stipulate the determination methods of 511 and 493 pesticides in milk, but these detection methods have sample pretreatment operations Complicated, large consumption of reagents and other issues
[0004] For methamidophos, chlormequat, cyromazine, imazapyr, aminopyralid and Aminocyclopyrachlor, the existing detection method removes the water in the sample, which is not conducive to the retention of the compound in the extraction solvent; it has passed the quantitative analysis and verification of the determination of the pesticide residue content in milk, and the method in the national standard is currently used for the determination of the residual content. The recovery rate is low, and the loss of the target is large, which affects the accuracy of the detection result

Method used

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  • Sample pretreatment and detection method for determining content of pesticide residues in cow milk
  • Sample pretreatment and detection method for determining content of pesticide residues in cow milk
  • Sample pretreatment and detection method for determining content of pesticide residues in cow milk

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1 Sample pretreatment and detection method for the determination of pesticide residues in milk

[0054] The reagents used in this embodiment are: acetonitrile (CH 3 CN), Methanol (CH 3 OH), all chromatographically pure, purchased from Merck Chemical Technology (Shanghai) Co., Ltd.; formic acid (HCOOH), mass spectrometry grade, purchased from Shijiazhuang Modern Instrument Chemical Co., Ltd.;

[0055] Pesticide standard products are: chlormequat, methamidophos, cyromazine, aminopyralid, clopromic acid and imazethapyr a total of 6 standard products, all purchased from Dr Ehrenstorfer in Germany;

[0056] Instrument materials include: Oasis HLB solid-phase extraction column; high performance liquid chromatography tandem mass spectrometer TQ-XS, Waters Technology Co., Ltd.; TGL-20M centrifuge, Shanghai Luxiangyi Centrifuge Instrument Co., Ltd.; RE311 rotary evaporator, Yama extension company.

[0057] This embodiment includes the following steps carried out in se...

Embodiment 2-6

[0108] Example 2-6 Sample pretreatment and detection method for determination of pesticide residue content in milk

[0109] Examples 2-6 are respectively a sample pretreatment and detection method for the determination of pesticide residues in milk. Their steps are basically the same as those in Example 1. The only difference lies in the process parameters and detection results. See the table for details. 6 and Table 7:

[0110] Table 6 embodiment 2-6 process parameters

[0111]

[0112]

[0113] Table 7 embodiment 2-6 detection result

[0114]

[0115]

[0116]

[0117] The detection results of the above examples show that the sample pretreatment and detection method for the determination of pesticide residues in milk according to the present invention have a suitable retention time, the R value of the obtained regression equation is effective, the detection effect is good, and it can be effective for six pesticide components at the same time detection.

Embodiment 7

[0118] Example 7 Effect Experiment of Sample Pretreatment and Detection Method for Determination of Pesticide Residue Content in Milk

[0119] This example is an effect experiment of sample pretreatment and detection method for the determination of pesticide residue content in milk, and is used to verify the determination effect of the detection method of the present invention.

[0120] Adopt the method in embodiment 1 to measure pesticide residue content (measured value) to standard working solution (concentration is theoretical value) respectively, calculate the rate of recovery of detection method of the present invention, result is as shown in table 8:

[0121] Table 8 Effect Experimental Measurement Results

[0122]

[0123]

[0124] The above results show that the recovery rate of each group is stable, showing that the sample pretreatment and detection method for the determination of pesticide residue content in milk have good detection effect, effectively solve th...

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Abstract

The invention discloses a sample pretreatment and detection method for determining the content of pesticide residues in cow milk. The method comprises the following steps of carrying out effective extraction by using formic acid-acetonitrile extracting solution in a sample pretreatment process, filtering by means of a solid-phase extraction column, evaporating to dryness, dissolving by using methanol water, loading on a high performance liquid chromatograph tandem mass spectrometer, and determining the content of pesticide residues such as chlormequat chloride, methamidophos, cyromazine, aminopyralid, aminocyclopyrachlor and imazapyr in the cow milk. According to the sample pretreatment and detection method, the problem that specific pesticide residue components are difficult to extract in cow milk sample detection is effectively solved by adding the formic acid-acetonitrile extracting solution in a reasonable proportion, the accuracy and the recovery rate are remarkably improved, and the method is suitable for detecting the content of pesticide residues in cow milk.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection methods, and relates to the determination of pesticide residue content in milk, in particular to sample pretreatment and detection methods for the determination of pesticide residue content in milk. Background technique [0002] Pesticide residues gradually accumulate in human food along with the supply and demand sequence of food nutrition in the food chain. More than 90% of the pesticide components entering the human body come from food chain accumulation. In addition, pesticide residues can also be ingested by the human body through the atmosphere and drinking water. As milk products are included in the daily diet of all age groups, the trace but long-term harm of residual pesticides in milk to the human body cannot be ignored. Control the pollution of pesticide residues in dairy products and accurately detect pesticide ingredients to ensure the safety of dairy products , is...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/7266G01N30/8675G01N2030/062
Inventor 齐晓茹白晓云苏运聪柴艳兵张耀广李兴佳夏卫东张敏姚启禛马晓冲王鸽
Owner JUNLEBAO DAIRY GRP CO LTD
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