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Sample pretreatment method for detection of organochlorine pesticide residue in food

A technology for pesticide residue detection and sample pretreatment, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of complex process, cumbersome operation, time-consuming, etc., achieve mild extraction conditions, solve cumbersome operations, and simple operation steps. Effect

Inactive Publication Date: 2012-07-11
YANTAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, through testing practice, it is found that this method is not only complicated in process, cumbersome in operation, time-consuming, but also not strong in purification ability.
In 2003, Lehotay and Anastassiadas proposed the QuEChERS (quick, easy, cheap, effective, rugged, and safe) pesticide multi-residue detection technology, which uses a dispersive solid-phase extraction (DSPE) purification method, directly adding PSA to the acetonitrile extract Adsorbent powder for purification; this method is simple, fast, and requires a small amount of reagents, but the purification effect for some complex matrices is not ideal, and for some pesticides with low polarity, the detection limit of the method is difficult to meet the requirements
The use of organochlorine pesticides in this new type of aqueous two-phase system has a large partition coefficient to achieve the extraction of pesticide residues in food, and there is no report on this aspect so far

Method used

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  • Sample pretreatment method for detection of organochlorine pesticide residue in food
  • Sample pretreatment method for detection of organochlorine pesticide residue in food
  • Sample pretreatment method for detection of organochlorine pesticide residue in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Extraction of organochlorine pesticide residues in fish meat

[0017] Weigh 5g of carp back meat that has been homogenized, add 6.5g of water (add water according to the water content of the sample, so that the total water content is 10g, usually the water content of fresh meat is 70%, just add 6.5g of water), and vortex. Three kinds of two-phase aqueous systems were used to extract it: method (1) adding 3.4g potassium acetate and 4g acetonitrile; method (2) adding 4.0g sodium acetate and 4.8g acetonitrile; method (3) adding 2.8g potassium fluoride and 4 g of acetonitrile. Vortex the system for 1min, then centrifuge at 3500rpm for 10min, transfer the supernatant to another centrifuge tube, add 1g of anhydrous magnesium sulfate and 0.1g of PSA solid particles, vortex for 1min, centrifuge at 3500rpm for 10min, and extract at 20-30°C , take the supernatant, gas chromatography sampling detection. Taking method (1) as an example, the chromatogram of the spiked f...

example 2

[0018] Example 2: Detection of organochlorine pesticide residues in eggs

[0019] Discard the shell of the egg, mix the egg white and egg yolk, set aside. Take 10g sample, add 2.5g water (add water according to the water content of the sample, so that the total water content is 10g, usually fresh egg water is 75%, just add 2.5g water), and use three kinds of two-phase system to extract it: Method (1) add 1.9g dipotassium hydrogen phosphate, 2.5g potassium phosphate and 1.6g isopropanol; method (2) add 4.6g dipotassium hydrogen phosphate and 3.0g 1,2-propanediol; method (3) add 7.0g phosphoric acid potassium and 3.0 g 1,2-pentanediol. Vortex for 1min, then centrifuge at 3500rpm for 10min, transfer the upper phase liquid to another centrifuge tube, add 1.5g anhydrous magnesium sulfate and 0.15g C18 solid particles respectively, vortex for 1min, centrifuge at 3500rpm for 10min, the extraction temperature is 20-30℃, Take the supernatant and inject gas chromatography for detectio...

example 3

[0020] Example 3: Detection of organochlorine pesticide residues in milk powder

[0021] Take 1g of milk powder (moisture content of milk powder is less than 5%, which can be ignored), and use three kinds of two-phase systems to extract it: method (1) add 2.0g of water, 0.5g of sodium chloride and 2.5g of acetone; method (2) ) by adding 6g of water, 1.6g of ammonium sulfate and 2.4g of acetone; method (3) by adding 5.5g of water, 0.5g of sodium sulfate and 4.0g of acetonitrile. Vortex for 1 min, then centrifuge at 3500rpm for 10min, transfer the supernatant to another centrifuge tube, add 1g of anhydrous magnesium sulfate and 0.1g of PSA solid particles respectively, vortex for 1min, centrifuge at 3500rpm for 10min, the extraction temperature is 20-30℃, take The supernatant was injected and detected by gas chromatography. Taking method (1) as an example, the chromatogram of the milk powder spiked sample is shown in image 3 , 14 kinds of organochlorine pesticide addition rec...

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Abstract

The invention discloses a sample pretreatment method for detection of organochlorine pesticide residue in food and is characterized by comprising the following steps: water is added to a food sample, sample solution is swirled, and then inorganic salt and hydrophilic organic solvent are added to the sample solution, the sample solution is swirled and shaken uniformly, the sample solution undergoes phase splitting after centrifugation at room temperature, the upper-phase liquid is purified through dispersion solid-phase extraction method, the extraction temperature is 20-30 DEG C, and finally the upper-phase liquid is detected by gas chromatography; and the mass percent of the inorganic salt accounts for 5%-35% of the total mass of the system, the mass percent of the hydrophilic organic solvent accounts for 10%-50% of the total mass of the system, and water is of the residual amount, and the total mass of the system is the mass sum of water contained in the sample, the added water, the inorganic salt and the hydrophilic organic solvent. According to the sample pretreatment method, a dual-water-phase system consisting of the hydrophilic organic solvent, the organic salt and water is utilized, the partition coefficient is increased by means of changing the types and concentrations of the organic solvent and the inorganic salt, and the organochlorine pesticide residue in the sample can be directly extracted at room temperature.

Description

[0001] Technical field: [0002] The invention relates to a sample pretreatment method in food safety testing, in particular to a sample pretreatment method for detecting organochlorine pesticide residues in food. Background technique: [0003] Organochlorine pesticides have significant insecticidal effects and were once the most widely used insecticides in various countries. my country produced and used organochlorine pesticides in large quantities in the 1950s and 1980s. Organochlorine pesticides are highly toxic, can affect the activity of animal enzymes, interfere with the endocrine system, significantly affect the reproductive function of animals, and have been proven to have teratogenic, carcinogenic, and mutagenic effects. Organochlorine pesticides have a relatively stable structure, are not easy to degrade in nature, and have a half-life of several years. They can enter the adipose tissue of organisms through bioaccumulation, so they pose a huge threat to the ecolog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 殷军港刘永明李慧芳
Owner YANTAI UNIV
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