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Method for extracting and purifying short-chain chlorinated paraffins in serum

A short-chain chlorinated paraffin and serum technology, applied in the field of analytical chemistry, can solve the problems of easy access to large-volume samples of serum, no short-chain chlorinated paraffin, etc., and achieve the effect of short-chain chlorinated paraffin, simple operation, and good purification effect

Inactive Publication Date: 2018-11-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there have been no reports of chlorinated paraffins in serum, which may be due to the fact that there is no mature pretreatment and detection method for short-chain chlorinated paraffins in serum, and serum is not as easy to obtain large-volume samples as breast milk

Method used

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  • Method for extracting and purifying short-chain chlorinated paraffins in serum
  • Method for extracting and purifying short-chain chlorinated paraffins in serum
  • Method for extracting and purifying short-chain chlorinated paraffins in serum

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preparation example Construction

[0032] Preparation of 2% basic silica gel: prepare 50g / L potassium hydroxide solution (weigh 5g potassium hydroxide and add 100mL distilled water), fully dissolve. Take 40mL of 50g / L potassium hydroxide solution and add 100g of silica gel (in a flat-bottomed flask), and shake fully until there is no adsorption at the bottom of the bottle and no agglomeration in the silica gel. Use a rotary evaporator to evaporate most of the water at 50°C, then increase the temperature from 50°C to 80°C, and dehydrate for 1 hour before use.

[0033] Active silica gel preparation: Silica gel (63-100 μm, Sunchrom, Germany), calcined in a muffle furnace at 550-650° C. for 4-12 hours, cooled in a desiccator for later use.

[0034] The preparation method of 44% acidified silica gel is as follows: put 200g of active silica gel and 157g of concentrated sulfuric acid in a brown bottle, fully shake it for 2-3 hours, and store it in a desiccator.

Embodiment 1

[0036] After centrifuging the whole blood, separate the serum, weigh 1g of serum, put it in a 10mL glass centrifuge tube, add 1mL of high-grade pure concentrated sulfuric acid, wait until the reaction is complete (remove protein and fat) and cool; add 1mL DCM, vortex ( XW-80A, 2800rpm) for 5min, centrifuged at 2000rpm for 10min, and the supernatant was transferred to a 250mL flat-bottomed flask. Repeat three times, concentrate the extract to about 1mL; fill the silica gel column from bottom to top: 5g anhydrous sodium sulfate, 2g 2% basic silica gel, 2g active silica gel, 5g acidified silica gel, 10g anhydrous sodium sulfate, discard 30mL after loading Hex eluate, followed by 50mL Hex / DCM (1:1, v / v) and 50mL Hex / DCM (1:2, v / v) eluate; 100mL eluate was concentrated to about 1mL and blown with nitrogen When it is nearly dry, use 20 μL of 50ppb 13C-α-HCH to make up the volume and analyze it with HRGC-ECNI-LRMS. Calculation results The concentration of short-chain chlorinated par...

Embodiment 2

[0038] After centrifuging the whole blood, separate the serum, weigh 1g of serum, put it in a 10mL glass centrifuge tube, add 1mL of high-grade pure concentrated sulfuric acid, wait for the reaction to complete and cool down; add 1mL hex, vortex (XW-80A, 2800rpm) 5min, centrifuge at 2000rpm for 10min, and transfer the supernatant to a 250mL flat-bottomed flask. Repeat three times, concentrate the extract to about 1mL; fill the silica gel column from bottom to top: 5g anhydrous sodium sulfate, 2g 2% basic silica gel, 2g active silica gel, 5g acidified silica gel, 10g anhydrous sodium sulfate, discard 30mL after loading Hex eluate, followed by 50mL Hex / DCM (1:1, v / v) and 50mL Hex / DCM (1:2, v / v) eluate; 100mL eluate was concentrated to about 1mL and blown with nitrogen When it is nearly dry, use 20 μL of 50ppb 13C-α-HCH to make up the volume and analyze it with HRGC-ECNI-LRMS. Calculation results The concentration of short-chain chlorinated paraffins was 40.7 ng per gram of seru...

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Abstract

The invention provides a method for extracting and purifying short-chain chlorinated paraffins in serum. The method includes steps of adding concentrated sulfuric acid into the serum, removing proteins and fat in the serum, further adding n-hexane and / or dichloromethane into the serum, carrying out vortex oscillation and carrying out centrifugation to obtain supernatant extract liquid; carrying out purification elution on the extract liquid by the aid of multilayer silica gel columns; concentrating effluent with the short-chain chlorinated paraffins, and then carrying out nitrogen blowing until the effluent is nearly dry so as to obtain the short-chain chlorinated paraffins in the serum. Fillers in the silica gel columns include anhydrous sodium sulfate, alkaline silica gel, activated silica gel, acidified silica gel and anhydrous sodium sulfate from bottom to top. The method has the advantages that serum samples treated by the aid of the method are analyzed by the aid of gas chromatography-electron capture negative chemical source / low-resolution mass spectrometry; extraction treatment is carried out on the SCCPs (short-chain chlorinated paraffins) in the serum for the first time,and the proteins and the fat are treated by sulfuric acid; the method is easy and convenient to operate and good in repeatability, and pretreatment methods can be provided to research on the SCCPs inthe serum and the human exposure levels.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a method for extracting and purifying short-chain chlorinated paraffins in serum. Background technique [0002] Chlorinated paraffins are a complex class of chlorinated alkanes containing more than 10,000 homologues and isomers. Commercial chlorinated paraffins are obtained by direct chlorination of n-alkanes, and their chlorine content is between 30% and 70%. Based on their chain length, they can be divided into short-chain chlorinated paraffins, medium-chain chlorinated paraffins and long-chain chlorinated paraffins. Chlorinated paraffins. Chlorinated paraffins are widely used in human production and life, such as lubricants, metal cutting fluids, flame retardants and plasticizers in PVC, rubber, coatings, pigments and sealants, etc. Studies have shown that chlorinated paraffins are persistent in the environment while being prone to long-distance transport in the atmosphere d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34
CPCG01N1/34
Inventor 陈吉平徐甲知张海军高媛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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