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Method for measuring pesticide residue quantity in leather

A technology for pesticide residues and leather, applied in the field of analytical chemistry, can solve the problems of no relatively perfect method, no standard method, etc.

Inactive Publication Date: 2009-08-05
通标标准技术服务(天津)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, there is no relatively perfect method for the detection of pesticide residues in leather, and there is no standard method to follow.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Example 1 Detection of pesticides in pigskin samples

[0047] 1. Extraction and purification

[0048] A. Extraction:

[0049] a. Weigh 5.0 g of sample mixed uniformly in a 150 mL beaker;

[0050] b. Add 50mL of n-hexane, mix thoroughly, and ultrasonicate for 60min in a water bath at 50°C, and filter the extract into a 250mL separatory funnel through filter paper;

[0051] c. Add 50 mL of acetonitrile to the sample residue, sonicate in a water bath at 50°C for 60 minutes, and combine the acetonitrile phase into a separatory funnel;

[0052] B. Purification:

[0053] a. Liquid-liquid extraction

[0054] The separatory funnel was shaken on the shaker for 30 minutes, and the acetonitrile layer was transferred to a flat-bottomed flask, and the n-hexane phase was extracted twice with 30 mL of acetonitrile by shaking for 40 minutes each time, and the acetonitrile phase was combined and put into a flat-bottomed flask;

[0055] The combined acetonitrile extract was concentr...

Embodiment 2

[0093] Example 2 Detection of Pesticide Residues in Cowhide Samples

[0094] 1. Extraction and purification

[0095] A. Extraction:

[0096] a. Weigh 3.0g sample which is mixed uniformly in a 150mL beaker;

[0097] b. Add 40mL of n-hexane, mix thoroughly, and ultrasonicate for 80min in a water bath at 60°C, and filter the extract into a 250mL separatory funnel through filter paper;

[0098] c. Add 40 mL of acetonitrile to the sample residue, sonicate in a water bath at 60°C for 80 minutes, and combine the acetonitrile phase into a separatory funnel;

[0099] B. Purification:

[0100] a. Liquid-liquid extraction

[0101] The separatory funnel was shaken on the shaker for 40 minutes, the acetonitrile layer was transferred to a flat-bottomed flask, and the n-hexane phase was extracted with 30 mL of acetonitrile by shaking for 3 times, each shaking for 30 minutes, and the acetonitrile phase was combined and put into a flat-bottomed flask;

[0102] The combined acetonitrile ex...

Embodiment 3

[0141] Example 3 Detection of Pesticide Residues in Sheepskin

[0142] 1. Extraction and purification

[0143] A. Extraction:

[0144] a. Weigh 5.0 g of sample mixed uniformly in a 150 mL beaker;

[0145] b. Add 50mL of n-hexane, mix thoroughly, and ultrasonicate for 60min in a water bath at 50°C, and filter the extract into a 250mL separatory funnel through filter paper;

[0146] c. Add 50 mL of acetonitrile to the sample residue, sonicate in a water bath at 50°C for 60 minutes, and combine the acetonitrile phase into a separatory funnel;

[0147] B. Purification:

[0148] a. Liquid-liquid extraction

[0149] The separatory funnel was shaken on the shaker for 30 minutes, the acetonitrile layer was transferred to a flat-bottomed flask, and the n-hexane phase was extracted with 30 mL of acetonitrile by shaking for 3 times, each shaking for 40 minutes, and the acetonitrile phase was combined and put into a flat-bottomed flask;

[0150] The combined acetonitrile extract was ...

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PUM

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Abstract

The invention relates to a combined gas chromatography mass spectrometry measuring method for measuring the pesticide residue in leather, which belongs to the field of analytical chemistry. The method adopts normal hexane and acetonitrile to perform ultrasonic extraction to a leather sample and separates and purifies the sample extracting solution by various means such as liquid-liquid extraction, gel permeation chromatograph, adsorbent chromatography column, solidoid extraction column, and the like by aiming to the characteristics that the leather sample has high oil content, the residual processing assistant is complex, and the like, and the pesticide residue of the processed sample extracting solution is measured by the combined gas chromatography mass spectrometry. The invention has the advantages of high selectivity, wide range of application and low detectability, realizes the measurement of the pesticide residue in the leather, creates a new thought for the measurement of the pesticide residue in the leather and fills in a gap for the measurement of the pesticide residue.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a method for measuring pesticide residues in leather by gas chromatography-mass spectrometry. It specifically involves ultrasonically extracting leather samples through n-hexane and acetonitrile, using liquid-liquid extraction, gel permeation chromatography (GPC), adsorbent chromatography column, solid phase extraction column (SPE column) to separate and purify pesticides in the sample extract, and gas chromatography - Determination of its content by mass spectrometry. Background technique [0002] Pesticides are widely used in agricultural production and industrial production. While playing their role in killing insects and bacteria, pesticides have also become one of the important pollutants. Pesticide residues in food and daily necessities invade the human body through digestive tract, respiratory tract and skin contact, thus causing damage to people's health. Different pes...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N27/64G01N30/06
Inventor 陈志强俞安敏李军王大章王培花李耀青
Owner 通标标准技术服务(天津)有限公司
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