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Pretreatment method for detecting organochlorine pesticide residue

A pesticide residue and organochlorine technology, applied in the field of pesticide science and testing, can solve the problems of vegetable export obstruction, human and animal poisoning, etc., and achieve the effects of less reagent volume, high precision and simple operation.

Inactive Publication Date: 2012-10-17
吴桂玲
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Every year in our country, incidents of human and animal poisoning caused by eating vegetables contaminated with highly toxic pesticides occur, and even the export of vegetables is blocked due to excessive pesticide residues

Method used

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  • Pretreatment method for detecting organochlorine pesticide residue
  • Pretreatment method for detecting organochlorine pesticide residue
  • Pretreatment method for detecting organochlorine pesticide residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 A pretreatment method for detecting organochlorine pesticide residues, comprising the following steps:

[0027] ⑴ Fresh green vegetables are beaten according to conventional methods to obtain the samples to be tested.

[0028] (2) Add 40mL of acetonitrile to 20g of the sample to be tested, homogenize at a rate of 8000r / min for 2min, then add 5g of dried NaCl into a 100mL centrifuge tube with a stopper, cover and shake vigorously for 2min, then Centrifuge at a speed of 4000 r / min for 2 min, and after standing at room temperature, obtain a supernatant; finally draw 5 mL of the supernatant into a concentrated bottle, and in an environment with a speed of 180-280 r / min and a water bath temperature of 30-40°C Use a rotary evaporator under certain conditions to evaporate until the remaining 1-2mL, and then dry it with an ear wash ball to obtain a concentrate.

[0029] (3) Add 10 mL of eluent to the concentrate to completely dissolve the concentrate to obtain s...

Embodiment 2

[0034] Example 2 A pretreatment method for detecting organochlorine pesticide residues, comprising the following steps:

[0035] (1) Fresh eggplants were beaten according to conventional methods to obtain samples to be tested.

[0036] (2) Add 50 mL of acetonitrile to 25 g of the sample to be tested, homogenize at a rate of 12000 r / min for 2 min, then add 6 g of dried NaCl into a 100 mL centrifuge tube with a stopper, cover it and shake vigorously for 3 min, then Centrifuge at a speed of 4000 r / min for 3 minutes, and after standing at room temperature, obtain the supernatant; finally pipette 10 mL of the supernatant into a concentrated bottle, at a speed of 180-280 r / min, and a water bath temperature of 30-40°C Use a rotary evaporator to evaporate to the remaining 1~2mL under certain conditions, and then dry it with an ear wash ball to obtain a concentrate.

[0037] (3) Add 10 mL of eluent to the concentrate to completely dissolve the concentrate to obtain solution A fo...

Embodiment 3

[0042] Example 3 A pretreatment method for detecting organochlorine pesticide residues, comprising the following steps:

[0043] (1) Fresh tomatoes were beaten according to conventional methods to obtain samples to be tested.

[0044](2) Add 60 mL of acetonitrile to 30 g of the sample to be tested, homogenize at a rate of 10,000 r / min for 3 min, then add 8 g of dried NaCl into a 150 mL centrifuge tube with a stopper, cover and shake vigorously for 3 min, Next, centrifuge at a speed of 5000 r / min for 4 minutes, and after standing at room temperature, obtain the supernatant; Under the condition of ℃, use a rotary evaporator to rotate to 1~2mL, and then dry it with an ear washing ball to obtain a concentrate.

[0045] (3) Add 15 mL of eluent to the concentrate to completely dissolve the concentrate to obtain solution A for use; the eluent refers to the mixture obtained by mixing acetonitrile and toluene at a volume ratio of 3:1.

[0046] (4) Use 10 mL of eluent to pre-was...

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Abstract

The invention relates to a pretreatment method for detecting organochlorine pesticide residue. The method comprises the steps of (1) pulping fresh vegetables and fruits to obtain a sample to be detected; (2) adding acetonitrile into the sample to be detected for blending, then adding dried NaCl, centrifuging, and standing at room temperature to obtain supernate, evaporating the supernate to obtain a concentrate; (3) adding leacheate into the concentrate, and completely dissolving to obtain a solution A; (4) prewashing an amino column or a graphitized carbon black-amino serial column by the leacheate, removing the leacheate, and pouring the solution A instantly; (5) conducting column chromatography on the solution A, then adding the leacheate, and collecting to obtain a solution B; (6) evaporating the elution solution B until the constant weight is achieved to obtain eluate, conducting constant volume on the eluate by normal hexane; and (7) filtering the eluate, adding the eluate into an automatic sample feeding bottle, and the detecting the eluate by a gas chromatography electron capture detector (ECD). According to the method, the simplicity and the rapidness are realized, the pesticide residues in the vegetables and the fruits are extracted, and the quantitative detection of the pesticide residues can be realized.

Description

technical field [0001] The invention relates to the technical field of pesticide science and detection, in particular to a pretreatment method for detecting organochlorine pesticide residues. Background technique [0002] Pesticide residues are "invisible killers" in vegetables. In recent years, with the improvement of people's living standards, the consumption of vegetables has increased year by year, and has become a potentially huge commercial market. In order to pursue economic interests, some vegetable farmers use a large amount of chemicals such as highly toxic and high residue pesticides, which has caused Excessive pesticide residues are common in vegetables. People are paying more and more attention to the problem of pesticide residues. Every year in our country, incidents of human and animal poisoning caused by eating vegetables contaminated by highly toxic pesticides occur, and even the export of vegetables is hindered due to excessive pesticide residues. Theref...

Claims

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Application Information

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IPC IPC(8): G01N30/12G01N30/02
Inventor 吴桂玲
Owner 吴桂玲
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