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Method for detecting residues of carbendazol and thiabendazole in fruit and vegetable juice by high performance liquid chromatography

A technology of high performance liquid chromatography and liquid chromatography, which is applied in the field of detection of carbendazim and thiabendazole residues in fruit and vegetable juices by high performance liquid chromatography, and can solve the problems of cumbersome extraction process, large dilution volume, and inaccurate determination results, etc. problems, to achieve high sensitivity and recovery, low pollution, and reduce operational hazards

Inactive Publication Date: 2016-06-22
中华人民共和国赤峰出入境检验检疫局
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, high-performance liquid chromatography and high-performance liquid chromatography-mass spectrometry are the most commonly used methods for determining the residues of carbendazim and thiabendazole in fruit and vegetable juices. Most of the pretreatment processes require the use of alkali to adjust the pH and then use organic solvents to extract the target. Compounds, such as using methanol, acetonitrile, ethyl acetate, etc. to extract and pass through the column, have the following disadvantages: the extraction process is cumbersome; the adjustment with lye results in a larger dilution volume and inaccurate measurement results; extraction with organic solvents is easy Causes environmental pollution, and due to the use of organic reagents, the detection personnel are more dangerous to work

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] S1. Weigh 10g of the sample to be tested in a 50mL centrifuge tube, add 20mL of turpentine derivatives, vortex for 1min in a rapid mixer, extract by ultrasonic wave for 10min, centrifuge at 3000r / min for 5min, transfer the supernatant to a 100mL vessel with 3gNaCl Add 20mL turpentine derivatives to a stoppered measuring cylinder and repeat the extraction once. Combine the extracts in a 100mL stoppered measuring cylinder, shake for 1min, let stand for 30min, transfer quantitatively to a 50mL beaker, place on a heating plate at 60°C and blow with nitrogen to dry it, add Soak in 2mL of 0.1mol / L hydrochloric acid and cover with tinfoil;

[0020] S2, the C 18 The column was conditioned with 5mL turpentine derivatives for pre-drenching. When the solvent level reached the surface of the column adsorption layer, pour the sample solution obtained in step S1 immediately, collect the eluate, and place it on an electric heating plate at 35°C and blow it with nitrogen to dry it;

...

Embodiment 2

[0024] S1. Weigh 30g of the sample to be tested in a 100ml centrifuge tube, add 20mL of turpentine derivatives, vortex in a rapid mixer for 2min, extract by ultrasonic wave for 15min, centrifuge at 3000r / min for 5min, transfer the supernatant to a 100mL vessel with 5gNaCl added Add 20mL turpentine derivatives to a stoppered measuring cylinder and repeat the extraction once. Combine the extracts in a 100mL stoppered measuring cylinder, shake for 1min, let stand for 30min, transfer quantitatively to a 50mL beaker, place on a heating plate at 60°C and blow with nitrogen to dry it, add Soak in 2mL of 0.1mol / L hydrochloric acid and cover with tinfoil;

[0025] S2, the C 18 The column was conditioned with 5mL turpentine derivatives for pre-drenching. When the solvent level reached the surface of the column adsorption layer, pour the sample solution obtained in step S1 immediately, collect the eluate, and place it on an electric heating plate at 35°C and blow it with nitrogen to dry ...

Embodiment 3

[0029] S1. Weigh 20g of the sample to be tested in a 100mL centrifuge tube, add 20mL of turpentine derivatives, vortex in a rapid mixer for 1.5min, ultrasonically extract for 10-15min, centrifuge at 3000r / min for 5min, and transfer the supernatant to a tube containing 4gNaCl Add 20mL turpentine derivatives to a 100mL stoppered measuring cylinder and repeat the extraction once. Combine the extracts in a 100mL stoppered measuring cylinder, shake for 1min, let stand for 30min, transfer quantitatively to a 50mL beaker, and place on a heating plate at 60°C under nitrogen blowing for nearly Dry, add 2mL of 0.1mol / L hydrochloric acid to soak, cover with tinfoil;

[0030] S2, the C 18 The column was conditioned with 5mL turpentine derivatives for pre-drenching. When the solvent level reached the surface of the column adsorption layer, pour the sample solution obtained in step S1 immediately, collect the eluate, and place it on an electric heating plate at 35°C and blow it with nitroge...

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Abstract

The invention discloses a method for detecting residues of carbendazol and thiabendazole in fruit and vegetable juice by high performance liquid chromatography. The method comprises the following steps: after mixing a sample to be detected with a turpentine derivative, carrying out ultrasonic extraction and centrifuging; then repeating extraction for one time, and combining extracting solutions; blowing the mixed extracting solution with nitrogen gas until the extracting solution is nearly dry; adding 2mL hydrochloric acid and soaking; covering with tin foil paper; after carrying out pre-spraying conditioning on a C18 column, pouring the obtained sample solution in; collecting eluent and putting the eluent on an electric heating plate; blowing the eluent with the nitrogen gas at 35 DEG C until the eluent is nearly dry; then making the volume constant with the hydrochloric acid until the volume is 2mL; filtering with a filter membrane and transferring into a sample feeding bottle; enabling the solution to pass through a chromatographic column SunFireTM C18 at the flow speed of 1.0mL / min; after finishing sample feeding and quantifying with an external standard method, detecting by adopting a liquid chromatograph. The method disclosed by the invention has the advantages of rapidness, simplicity, high sensitivity and recovering ratio and small pollution; the used reagents are relatively environmentally friendly, and dangers to the working of detectors can be remarkably reduced.

Description

technical field [0001] The invention relates to the field of pesticide residue detection, in particular to a method for detecting carbendazim and thiabendazole residues in fruit and vegetable juices by high performance liquid chromatography. Background technique [0002] Carbendazim and Thiabendazole are high-efficiency and low-toxic benzimidazole broad-spectrum fungicides, which have control effects on various crop diseases caused by fungi (such as Deuteromycetes, Polyascomycetes), and have low toxicity to humans and animals. But in some countries, this fungicide can only be used on golf courses or recreational facilities, not on agricultural products. Relevant medical studies have shown that fungicides will increase the chances of animals suffering from liver tumors. The Coca-Cola carbendazim incident in the United States in 2012 drew greater attention to broad-spectrum fungicides. [0003] At present, the detection methods of carbendazim and thiabendazole mainly include...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 姜兆兴李智瑾王智亮曹旭赵敏任立新杨艳红赵静张鹏翔杨春燕
Owner 中华人民共和国赤峰出入境检验检疫局
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