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A method for determining the content of 4,4'-thiobisphenol in milk

A thiodiphenol and milk technology, which can be used in measuring devices, instruments, scientific instruments, etc., can solve problems such as 4,4'-thiodiphenol residues, achieve short time consumption, ensure food safety and physical health, Good precision and accuracy

Inactive Publication Date: 2018-12-04
LANZHOU INST OF ANIMAL SCI & VETERINARY PHARMA OF CAAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

4,4'-thiobisphenol in the environment is deposited on the surface of pasture through atmospheric circulation and water circulation, and dairy cows eat pasture containing 4,4'-thiobisphenol, which will directly cause 4,4'-thiodiphenol Phenol causes residues in milk, and if people consume milk containing this substance, it will cause serious consequences

Method used

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  • A method for determining the content of 4,4'-thiobisphenol in milk
  • A method for determining the content of 4,4'-thiobisphenol in milk

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Embodiment 1

[0021] 1. Sample pretreatment

[0022] Accurately weigh 2±0.02g of the milk sample, put it into a stoppered centrifuge tube, add 5ml of acetonitrile, 5ml of pure water and 0.5g of sodium chloride, cover the centrifuge tube, and place it in a 35°C water bath shaker for 30min. Centrifuge at a speed of 5000r / m for 10min, and transfer the upper acetonitrile layer to a 15ml centrifuge tube. Add 5ml of acetonitrile-saturated n-hexane, shake and extract for 10min, centrifuge at 5000r / m for 10min, suck out the upper n-hexane layer, dry the lower layer with acetonitrile and nitrogen, add 1ml of acetonitrile aqueous solution (v:v=45:55), vortex mix 30s, inhale into a 1ml syringe, filter through a 0.22μm composite filter, and set aside.

[0023] 2. Analytical and testing instrument conditions

[0024] Put the sample processed in step (1) on a high-performance liquid chromatograph (Waters 2695 type, equipped with a secondary integrated tube detector, Waters, USA) for determination, and ...

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Abstract

The invention discloses a method for determining 4, 4'-sulfo-diphenol content in milk. The method includes the steps of firstly, using an acetonitrile-salt-water mixing system to perform oscillation extraction on the milk, and separating after the extraction to obtain acetonitrile phase; secondly, using acetonitrile-saturated normal hexane to degrease the acetonitrile phase obtained in the first step, and performing volatilization drying on the degreased acetonitrile phase; thirdly, dissolving the sample obtained after the volatilization drying in the second step with an acetonitrile aqueous solution, filtering with a membrane, and using high performance liquid chromatograph to detect the filtrate, wherein the chromatographic conditions include, a C18 column is used, detection wavelength is 220-260 nanometers and flow phase is acetonitrile and water. The method has the advantages that the method is good in extraction effect, low in time consumption, good in sensitivity, precision and accuracy, applicable to the fast detection and screening of 4, 4'-sulfo-diphenol in milk samples, and the like, quality and safety monitoring requirements of the 4, 4'-sulfo-diphenol in the milk can be satisfied, and food safety and health of vast consumers are guaranteed.

Description

technical field [0001] The invention belongs to the field of food safety, and in particular relates to a method for determining the content of 4,4'-thiobisphenol in milk. Background technique [0002] 4,4'-Dihydroxydi-phenyl sulfide is an environmental hormone, CAS:2664-63-3, English name: 4,4'-Dihydroxydi-phenyl sulfide; 4,4'-Thiobisphenol, EINECS:220-197-9 , molecular formula: C 12 h 10 o 2 S, molecular weight: 218.27, structural formula: . In recent years, when the wave of industrialization has brought material civilization to human beings, people have discovered that 4,4'-thiobisphenol and other hormones that exist outside the biological body pass through soil, water, food chains, etc. due to industrial pollution and other reasons. way into the body of the residents. This substance will cause great harm to the human body, such as the reduction of sperm in men, male degeneration, and even the high incidence of male infertility; if women of childbearing age are poll...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 熊琳阎萍李维红高雅琴杨晓玲
Owner LANZHOU INST OF ANIMAL SCI & VETERINARY PHARMA OF CAAS