HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) detection method of 4-hexylresorcinol in crustacean aquatic products

A hexylresorcinol and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of insufficient qualitative ability, achieve high stability, less sample matrix interference, and good reproducibility

Inactive Publication Date: 2018-01-12
ZHEJIANG ECONOMIC & TRADE POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The detection limit of gas chromatography (GC-FID) cannot meet the requirements of the standard, and the detection limit of liquid chromatography fluorescence detection can meet the requirements, but due to its insufficient qualitative ability, there are certain limitations to some extent. defect

Method used

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  • HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) detection method of 4-hexylresorcinol in crustacean aquatic products
  • HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) detection method of 4-hexylresorcinol in crustacean aquatic products
  • HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) detection method of 4-hexylresorcinol in crustacean aquatic products

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Experimental program
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Embodiment

[0052] 1. Detection technology scheme

[0053] 1 scope of application

[0054] Using shrimp and other aquatic products (shrimp, crab) as the substrate, a method for the determination of 4-hexylresorcinol (4-HR) residues by ultra-high performance liquid chromatography tandem mass spectrometry was determined.

[0055] 2 detection principle

[0056] Use acetonitrile and dichloromethane (7+3) to extract the residual 4-hexylresorcinol in the sample, spin the extract to nearly dryness and dissolve it with dichloromethane, clean it with an amino solid-phase extraction column, dissolve it with a mobile phase, and enter Mass spectrometry, external standard method for quantification.

[0057] 3 Sample pretreatment

[0058] 3.1 Extraction

[0059] Weigh 5g (accurate to 0.01g) of the sample into a 50mL centrifuge tube, add 10mL of acetonitrile and dichloromethane solution, homogenize with a high-speed tissue grinder for 2min, cap the plug, vortex mix for 1min, ultrasonically extract f...

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Abstract

The invention relates to the technical field of detection of chemical substances and in particular relates to an HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometry)detection method of 4-hexylresorcinol in crustacean aquatic products. The HPLC-MS/MS detection method comprises the following steps: extracting residual 4-hexylresorcinol in a sample to be detected by utilizing a mixed solution of acetonitrile and dichloromethane; carrying out rotary evaporation on an extracting solution until the extracting solution is nearly dry; then dissolving by utilizing dichloromethane; purifying by utilizing a solid-phase extraction column and dissolving by utilizing a mobile phase; detecting through a high performance liquid chromatography-mass spectrometry system. The invention establishes a pre-treatment method which is suitable for sample extraction, purification and concentration and ensures that matrix interferences on the sample in an analysis and determination process are minimum; chromatography-mass spectrometry conditions are optimized to finally determine external standard method quantification. According to the method provided by the invention, thequantification limit is 4mu g/kg and the standard recovery rate under each concentration is 70 percent or more.

Description

technical field [0001] The invention relates to the technical field of chemical substance detection, in particular to an HPLC-MS / MS detection method for 4-hexylresorcinol in crustacean aquatic products. Background technique [0002] Penaeus vannamei Boone, scientific name Litopenaeus vannamei. There are many areas in my country where Penaeus vannamei is cultured. Among them, the aquaculture area of ​​Penaeus vannamei in Hangzhou was 103,000 mu in 2013. In 2013, the total output of Penaeus vannamei in the city reached 34,000 tons. It is one of the largest and pillar aquaculture products in Hangzhou. . [0003] Penaeus vannamei contains rich nutrients such as protein, trace elements and physiological activities. The taste produced by its unique taste substances is very consistent with people's best taste. It tastes delicious, but the crustaceans are easy to blacken. After it is captured, a series of biochemical reactions are accelerated by polyphenol oxidase (PPO) in the body...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 叶素丹郝云彬阙斐陈岭冯文婕
Owner ZHEJIANG ECONOMIC & TRADE POLYTECHNIC
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