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Method for simultaneously determining residual organochlorine, pyrethroid and organophosphorus pesticides in food

A technology of organochlorine and organophosphorus, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of increased workload, waste of reagents and processing time, long analysis cycle, etc., achieve good separation, simple measurement, reduce Effects of Organic Reagent Consumption

Inactive Publication Date: 2015-07-08
TIANJIN TIANSHI BIOLOGICAL DEV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this detection method are: the use of different pretreatment methods wastes reagents and processing time, the use of different instrument conditions increases the workload and the analysis cycle is long

Method used

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  • Method for simultaneously determining residual organochlorine, pyrethroid and organophosphorus pesticides in food
  • Method for simultaneously determining residual organochlorine, pyrethroid and organophosphorus pesticides in food
  • Method for simultaneously determining residual organochlorine, pyrethroid and organophosphorus pesticides in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for simultaneously determining residual organochlorines, pyrethroids and organophosphorus pesticides in food, comprising the steps of:

[0020] (1) Weigh 10 g of the sample to be tested, add 20 ml of petroleum ether and shake and extract for 20 minutes; separate the petroleum ether extract, then shake and wash with 10 ml of petroleum ether, wash twice, shake for 5 minutes each time; separate the petroleum ether washing liquid, and The petroleum ether washing liquid and the petroleum ether extract were combined to form a combined liquid, and the combined liquid was rotary evaporated to a volume of 1 mL, and 2 mL of petroleum ether was added to dissolve it, and then it was purified by a Florisil solid-phase extraction column, and was extracted with n-hexane-ethyl acetate 4 mL of the solution was eluted to obtain an eluate;

[0021] (2) Take another 10 g of the sample to be tested, add 20 ml of acetone and shake and extract for 30 minutes; separate the acetone ext...

Embodiment 2

[0032] A method for simultaneously determining residual organochlorines, pyrethroids and organophosphorus pesticides in food, comprising the steps of:

[0033] (1) Weigh 10g of the sample to be tested, add 15ml of petroleum ether and shake and extract for 10min; separate the petroleum ether extract, then shake and wash with 15ml of petroleum ether, wash twice, shake for 3min each time; separate the petroleum ether washing liquid, and The petroleum ether washing liquid and the petroleum ether extract were combined to form a combined liquid, and the combined liquid was rotary evaporated to a volume of 1 mL, and 2 mL of petroleum ether was added to dissolve it, and then it was purified by a Florisil solid-phase extraction column, and was extracted with n-hexane-ethyl acetate 4 mL of the solution was eluted to obtain an eluate;

[0034] (2) Another 10 g of the sample to be tested was weighed, and 15 ml of acetone was added to shake and extract for 30 minutes; the acetone extract w...

Embodiment 3

[0040] A method for simultaneously determining residual organochlorines, pyrethroids and organophosphorus pesticides in food, comprising the steps of:

[0041] (1) Weigh 10 g of the sample to be tested, add 20 ml of petroleum ether and shake and extract for 30 minutes; separate the petroleum ether extract, then shake and wash with 10 ml of petroleum ether, wash 3 times, shake for 5 minutes each time; separate the petroleum ether washing liquid, and The petroleum ether washing liquid and the petroleum ether extract were combined to form a combined liquid, and the combined liquid was rotary evaporated to a volume of 1 mL, and 2 mL of petroleum ether was added to dissolve it, and then purified by a Florisil solid-phase extraction column, and the mixture was purified with n-hexane-ethyl acetate 4 mL of the solution was eluted to obtain an eluate;

[0042] (2) Take 10g of the sample to be tested, add 20ml of acetone and shake and extract for 30min; separate the acetone extract, the...

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Abstract

The invention discloses a method for simultaneously determining residual organochlorine, pyrethroid and organophosphorus pesticides in food. The method comprises the following steps of: (1) taking a sample to be tested and adding petroleum ether for extraction, separating out the extract liquid, washing by using petroleum ether, blending the washing liquid with the extract liquid, evaporating, dissolving in petroleum ether, purifying through Florisil solid-phase extraction column, and eluting to obtain eluate; (2) further weighing the sample to be tested and adding acetone for extraction, separating out the extract liquid, further washing by using acetone, blending the washing liquid with the extract liquid, evaporating, and determining the constant volume by using acetone; (3) taking the liquid obtained in the step (1) and the liquid obtained in the step (2), injecting the mixed liquid in a gas chromatograph, analyzing the sample by simultaneously using a double-capillary chromatographic column, employing consistent stage-by-stage temperature rise conditions, simultaneously performing respective analysis, and feeding the sample into an electron-capture detector and a pulse flame photometric detector after separation through two chromatographic columns, respectively. The method disclosed by the invention is simple and convenient, quick and accurate in determination, good in reproducibility and high in accuracy rate.

Description

technical field [0001] The invention relates to a method for simultaneously determining residual organochlorine, pyrethroid and organophosphorus pesticides in health food. Background technique [0002] my country is a big country in the production and use of pesticides. In agricultural production, organochlorine, organophosphorus and pyrethroids are the three most commonly used pesticides. Organophosphorus pesticides are generally highly toxic and easily attached to leaves, flowers, fruits and other parts of plants. ; Organochlorine pesticides have good stability. The famous HCH and DDT can exist stably in the soil for more than 60 years; pyrethroid pesticides are more and more widely used pesticides in recent years, some of which have low toxicity, high efficiency, and easy decomposition However, fenvalerate, deltamethrin and other varieties are extremely toxic and have been included in the category of prohibited pesticides. [0003] Organophosphorus pesticides can enter the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 赵晓娟李星芝陈绪卓
Owner TIANJIN TIANSHI BIOLOGICAL DEV