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An extraction and purification method for the analysis of organochlorine pesticides in marine shellfish tissue

An organochlorine and shellfish technology, which is applied in the field of extraction and purification of organochlorine pesticide analysis, can solve the problems of no application, promotion value, structural damage of target compounds, and high instrument requirements, and achieves low cost, good peak shape, and matrix interference. less effect

Inactive Publication Date: 2015-08-05
余新威
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] High instrument requirements (GPC purification), high operating costs, long time-consuming (GPC purification, Soxhlet extraction), structural damage to some target compounds (concentrated H 2 SO 4 Pickling to remove fat, protein) and other shortcomings, does not have very good application and promotion value

Method used

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  • An extraction and purification method for the analysis of organochlorine pesticides in marine shellfish tissue
  • An extraction and purification method for the analysis of organochlorine pesticides in marine shellfish tissue
  • An extraction and purification method for the analysis of organochlorine pesticides in marine shellfish tissue

Examples

Experimental program
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Effect test

Embodiment 1

[0022] An extraction and purification method for the analysis of organochlorine pesticides in marine shellfish tissue, comprising the following steps: adding 5ml of ultrapure water and 10ml of extract to centrifuge tube 1, adding 0.5-1.0ug ISTD internal standard mixed solution and 0.2- 0.5ug 13 C 12 -PCB103 solution; wherein the composition of the extract is weight percentage: 50% acetonitrile, 30% dichloromethane, 15% tetrahydrofuran, 5% D-type optical isomer of α-alanine; the tissue sample passes through 3000~4000rpm Homogenize for 60s, then add 10ml of pre-weighed mixed salt solution and 1-2ml of 30% phosphoric acid aqueous solution, shake for 5-10min, centrifuge at 3000rpm-4000rpm for 6-8min, draw about 5ml of supernatant through a syringe, Place in ~-26°C refrigerator for 2~3 hours, add centrifuge tube 1; the mixed salt contains 4~6g potassium sulfate, 1-2g sodium acetate, 1.0g sodium dihydrogen citrate; at the same time, add centrifuge tube 2 1-2g of magnesium chloride...

Embodiment 2

[0028] Different from Example 1, the mixed salt of this program is an aqueous solution containing 4g potassium sulfate, 1g sodium acetate, 1.0g sodium dihydrogen citrate, and 2ml of 30% phosphoric acid aqueous solution.

Embodiment 3

[0030] Different from Example 1, the mixed salt of this program is an aqueous solution containing 6g of potassium sulfate, 1g of sodium acetate, 1.0g of sodium dihydrogen citrate, and 1ml of 30% aqueous phosphoric acid.

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Abstract

The invention relates to an extraction and purification method for analyzing OCPs in marine shellfish tissue. The extraction and purification method comprises the steps of putting 5.0g of tissue sample in a centrifuge tube I, adding 5ml of ultrapure water and 10ml of extracting solution, and adding 0.5-1.0 microgram of internal standard mixed liquor and 0.2-0.5 microgram of 13C12-PCB103 solution, wherein the extracting solution comprises 50wt% of acetonitrile, 30wt% of dichloromethane, 15wt% of tetrahydrofuran, and 5wt% of D-type optical isomer of alpha-alanine; adding 10ml of mixed saline solution and 1ml-2ml of 30% phosphoric acid water solution into the centrifuge tube I; and adding 1g-2g of magnesium chloride into a centrifuge tube II, injecting 5ml of supernatant I in the centrifuge tube II, oscillating for 20s-30s, centrifuging for 10min-15min so as to obtain supernatant, and transferring the obtained supernatant into a gas chromatographic analysis bottle for instrument analysis. According to the extraction and purification method, the recovery rate of organochlorine ranges from 90% to 110% and is improved by more than 10% compared with that of a traditional scheme. The extraction and purification method has the advantages of slight matrix interference and good peak pattern and is favorable for inspection with a gas chromatograph or a gas chromatograph-mass spectrometer.

Description

technical field [0001] The invention relates to an extraction and purification method for the analysis of organochlorine pesticides in marine shellfish tissues. Background technique [0002] Organochlorine pesticides (OCPs) are one of the 12 priority organic pollutants, which have been widely produced and used around the world. As global pollutants, OCPs have long-term residual, bioaccumulative, semi- Volatile and highly toxic, OCPs have posed serious hazards to human health and the environment, and the determination of their residues in various samples has always been a research hotspot. [0003] Chinese patent document CN1563976 discloses a synchronous purification and extraction method for the analysis of organochlorine and organophosphorus pesticides, which has the advantages of less reagents used, higher safety, and fewer steps but can analyze more organochlorine and organophosphorus pesticides , where the recovery rate of organochlorine pesticides can reach more than ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 余新威胡灏琰方力王婕妤
Owner 余新威