Liquid chromatography tandem mass spectrometry detection method for measuring phthalates plasticizer in aquatic processing product

A medium phthalate, liquid chromatography technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to meet the rapid and advanced analysis technology, hinder the census of phthalate pollutants, consume large organic solvents, etc. High extraction efficiency and target yield, low equipment requirements, and simple and easy-to-control operations

Active Publication Date: 2019-04-09
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods are generally cumbersome and expensive to operate, and the sample pretreatment is complicated, inefficient, time-consuming, and consumes a large amount of organic solvents, often accompanied by secondary pollution caused by reagent

Method used

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  • Liquid chromatography tandem mass spectrometry detection method for measuring phthalates plasticizer in aquatic processing product
  • Liquid chromatography tandem mass spectrometry detection method for measuring phthalates plasticizer in aquatic processing product
  • Liquid chromatography tandem mass spectrometry detection method for measuring phthalates plasticizer in aquatic processing product

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Experimental program
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Effect test

Embodiment 1

[0030] A liquid chromatography tandem mass spectrometry detection method for the determination of phthalate plasticizers in processed aquatic products, including organic extraction, chromatographic purification, detection and analysis, in which the phthalic acid in processed aquatic products is extracted through the combination of extractant and dispersant Ester plasticizer, the above dispersant is tetrabutylammonium chloride and 4-hexyl resorcinol. This method is based on ultra-high performance liquid chromatography-mass spectrometry to detect and quantitatively analyze phthalate plasticizers extracted from processed aquatic products. This method has high sensitivity, high accuracy, and high throughput, and can be used in aquatic processing. Detection of phthalate plasticizers in products.

[0031] The organic extraction steps are as follows: take the dried edible part of the aquatic product processed Antarctic krill to make meat emulsion, add the extractant and the dispersant t...

Embodiment 2

[0041] A liquid chromatography tandem mass spectrometry detection method for determining phthalate plasticizers in processed aquatic products includes the following specific steps:

[0042] 1) Organic extraction: After the dried edible part of the processed aquatic product Antarctic krill is made into meat emulsion, the extractant is 1.2 times the weight of the processed aquatic product and the dispersant is 0.18 times the weight of the processed aquatic product. The mixture is vortexed for 4 minutes, and then the power is 200W. Under the conditions of ultrasonic extraction for 8 minutes, centrifuge at a rate of 8000r / min for 5 minutes to take the supernatant. After repeated extractions twice, the extract was evaporated and concentrated to 1 / 3 times the volume at 40°C to obtain the sample solution. The agent is a dichloromethane-n-hexane (1:1) mixed solvent, and the weight ratio of tetrabutylammonium chloride and 4-hexylresorcinol in the above dispersant is 2:4.3;

[0043] 2) Chrom...

Embodiment 3

[0046] A liquid chromatography tandem mass spectrometry detection method for the determination of phthalate plasticizers in processed aquatic products. The chromatographic purification steps are optimized. The specific optimization measures are as follows: the glass is chromatographed and the weight ratio is 1:1. Packed with neutral alumina and anhydrous sodium sulfate. After rinsing with n-hexane, transfer the sample solution to the chromatography column at a flow rate of 1.5 mL / min, and then use the same amount of dichloromethane-n-hexane mixed solution and acetic acid Elute with ethyl acetate-n-hexane mixed solution at a flow rate of 2.5mL / min. Collect the sample effluent and the target eluate, rotate and evaporate at 35~45℃ to obtain the solid phase, and then dissolve it with methanol to a constant volume. 1~2mL, pass through a 0.22μm microporous membrane for use. The volume ratio of the components in the methylene chloride-n-hexane mixed solution is dichloromethane: n-hexan...

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Abstract

The invention provides a liquid chromatography tandem mass spectrometry detection method for measuring a phthalates plasticizer in an aquatic processing product, and belongs to the technical field ofproduct safety and detection. The method comprises the following steps: extracting the phthalates plasticizer in the aquatic processing product through the matching of an extraction agent and a dispersing agent; after purifying and eluting a sample solution obtained by extracting, detecting the sample solution by using an ultra-high performance liquid chromatography tandem mass spectrometry; and the dispersing agent is tetrabutylammonium chloride and 4-hexylresorcinol. According to the liquid chromatography tandem mass spectrometry detection method for measuring the phthalates plasticizer in the aquatic processing product provided by the invention, a pretreatment process is high in target selectivity and enrichment factor and good in operation repeatability, small in solvent dosage, strongin purification effect, wide in linear range of a measurement result, high in accuracy, high in target ion determination specificity and sensitivity, high in sample purity and stability, small in matrix interference, strong in practicability, and has the application of detecting the phthalates plasticizer in the aquatic processing product.

Description

Technical field [0001] The invention belongs to the technical field of product safety and detection, and specifically relates to a liquid chromatography tandem mass spectrometry detection method for determining phthalate plasticizers in processed aquatic products. Background technique [0002] Phthalate ester plasticizers (PAEs) are a kind of environmental hormones with carcinogenicity, mutagenicity, teratogenicity, reproductive toxicity, neurotoxicity, endocrine disrupting properties, mostly colorless oily viscous liquid, easily soluble Fat and organic solvents are hard to dissolve in water and are not easily volatile. They contain weaker estrogen components, especially the bioaccumulation of long-chain phthalates and the potential carcinogenic risk, as well as the destructive effect on the secretion of biological hormones. It destroys the immune system and causes reproductive toxicity and has the ability to gradually enter the food chain. Internationally, research on phthalate...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 方益何鹏飞严忠雍李佩佩
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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