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Extraction method for residual pyrethroid pesticides in water environment

A pyrethroid, water environment technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of high price, poor selectivity, reduced detection sensitivity, etc., and achieve the effect of fast separation

Inactive Publication Date: 2012-06-20
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, solid-phase extraction needs to consume a certain amount of organic solvents, especially before performing solid-phase extraction, it is usually necessary to perform LLE to separate the target from the complex matrix, which further increases the consumption of organic solvents and operating steps, and reduces the detection efficiency. sensitivity
Micro-extraction technology has become an important development trend. For example, SPME is a micro-extraction technology developed on the basis of solid-phase extraction technology. It has the advantages of short operation time, small sample volume, and no need for extraction solvents. However, it is expensive and the type of coating Limited and poor selectivity; SBSE has a similar adsorption mechanism to SPME, has a relatively thick polymer adsorption layer, and has a higher adsorption factor, but also has the disadvantages of limited coating types and expensive prices. application is constrained

Method used

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  • Extraction method for residual pyrethroid pesticides in water environment
  • Extraction method for residual pyrethroid pesticides in water environment
  • Extraction method for residual pyrethroid pesticides in water environment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Use a density of 0.02mm as the density of 0.915 g / cm 3 A low-density polyethylene film was used to prepare an extraction film bag with an inner diameter of 4 mm and a length of 2 cm.

[0022] Soak the extraction film bag in a mixed solution of n-hexane and acetone with a volume ratio of 9:1 for 10 minutes to pretreat the film bag.

[0023] Take 15ml of water sample, add appropriate amount of sodium chloride until the solution is saturated, and place the saturated solution in a 20ml headspace sampling vial.

[0024] Fix the above-mentioned film bag in the headspace sample bottle, then add 0.2ml of n-hexane into the film bag, and seal it with a cap. Then the headspace vial was placed in a shaker and extracted at 25°C and 300rpm for 180min.

[0025] After the extraction, the extraction solvent was transferred to a 2.0ml sample injection vial and detected by GC-ECD. The detection results are shown in Table 1, and the chromatogram is shown in Table 1 figure 1 shown.

[0...

Embodiment 2

[0031] With a density of 0.03mm is 0.920 g / cm 3 A low-density polyethylene film was used to prepare an extraction film bag with an inner diameter of 5 mm and a length of 3 cm.

[0032] Soak the extraction film bag in a mixed solution of n-hexane and acetone with a volume ratio of 9:1 for 15 minutes to pretreat the film bag.

[0033] Take a 15ml water sample, add appropriate amount of sodium chloride to a saturated solution, and place it in a 20ml headspace sampling vial.

[0034] Fix the above membrane bag in the headspace sampling bottle, then add 0.4ml cyclohexane into the membrane bag, and seal the top hole sampling bottle with a cap.

[0035] The headspace sampling vial was placed in a shaker and extracted at 30°C and 450rpm for 120min.

[0036] After the extraction was finished, the extraction solvent was transferred to a 2.0ml sample injection vial and detected by GC-MS. The results are shown in Table 2 and figure 2 shown.

[0037] Table 2 GC-MS analysis results of ...

Embodiment 3

[0041] With a density of 0.04mm is 0.930 g / cm 3 A low-density polyethylene film was used to prepare an extraction film bag with an inner diameter of 6 mm and a length of 4 cm.

[0042] Soak the extraction film bag in a mixed solution of n-hexane and acetone with a volume ratio of 9:1 for 12 minutes to pretreat the film bag.

[0043] Take a 15ml water sample, add appropriate amount of sodium chloride to a saturated solution, and place it in a 20ml headspace sampling vial.

[0044] Fix the above-mentioned film bag into the headspace sampling bottle, then add 0.8ml of n-hexane into the film bag, and seal the headspace sample bottle with a cap.

[0045] The headspace vial was placed in a shaker and extracted at 45°C and 600rpm for 60min.

[0046] After the extraction is finished, the extraction solvent is transferred to a 2.0ml sample injection vial and detected by GC-MS. The inventive effect is similar to that of Example 2.

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Abstract

The invention relates to an extraction method for residual pyrethroid pesticides in a water environment, which is characterized by pretreating a low-density polyethylene extraction membrane bag placed into normal hexane and acetone mixture liquor; adding sodium chloride into a sample to be detected until saturated concentration and placing a saturated liquor sample in a headspace sample injectionbottle; fixing the pretreated membrane bag into the headspace sample injection bottle added with the saturated liquor sample, adding extraction solvents into the membrane bag, sealing the headspace sample injection bottle and placing the headspace sample injection bottle in an oscillator to obtain extraction liquor; and transferring the extraction liquor to a small sample injection bottle and measuring the concentration of the pyrethroid pesticides in the extraction liquor by the aid of a GC-ECD (gas chromatography-electron capture detector) or a GC-MS (gas chromatography-mass spectrometer). Compared with the prior art, a membrane-assisted extraction system obtained by means of research and development can be applied to separating and purifying the residual pyrethroid pesticides such as cypermethrin, deltamethrin, fluralinate, bifenthrin, phenothrin, fenvalerate and the like in the water environment sample. Compared with common liquid-liquid extraction and solid extraction methods, the extraction method is higher in separation speed and more efficient in enrichment of the pyrethroid pesticides.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and pesticide residue detection in water environment, and specifically refers to an extraction method for residual pyrethroid pesticides in water environment. Background technique [0002] Pyrethroid insecticides are a class of high-efficiency and broad-spectrum pesticides with low toxicity, rapid excretion and biodegradability. Therefore, they are often used in fishery production to kill parasites and harmful organisms. However, pyrethroid pesticides are highly toxic to aquatic organisms such as fish, shellfish and crustaceans, and recent studies have shown that the pesticides have a certain accumulation and are easily enriched by aquatic organisms, and some species have carcinogenic, teratogenic, Mutagenic and neurotoxic. In recent years, there have been frequent incidents of pollution and the death of aquaculture organisms. The use of such pesticides has had a serious impact on the water e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 史西志孙爱丽李德祥刘菁华陈炯
Owner NINGBO UNIV
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