A pretreatment method for the analysis of tetrabromobisphenol A in feces after biological poisoning
A tetrabromobisphenol and biological technology, which is applied in the field of detection and analysis of organic pollutants in biological samples, can solve problems such as persistent organic pollution, and achieve the effects of reducing matrix interference, good purification effect, and high recovery rate
Inactive Publication Date: 2015-10-21
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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In recent years, Tetrabromobisphenol A has been considered as a potential endocrine disruptor worthy of discussion and attention. Some studies also believe that Tetrabromobisphenol A has potential environmental persistence and bioaccumulation, which may cause persistent organic pollution problems
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[0025] The technical solution of the present invention will be further described below in conjunction with the embodiments.
[0026] (1) Extraction and purification of feces
[0027] After collecting fecal samples from biological exposure and poisoning, impurities were picked out with tweezers, freeze-dried, ground and pulverized. Accurately weigh the dried stool sample, add 15mL equal volume of mixed methyl tert-butyl ether and n-hexane reagent, ultrasonically extract for 30 minutes with an ultrasonic cleaner, and then centrifuge for 5 minutes at a speed of 3000 rpm in a centrifuge. Remove the upper extract and repeat three times; combine the three extracts, dry over anhydrous sodium sulfate, and dilute to 50 mL; pipette 20 μL into the well-mixed extract, add 10 ng C13-labeled tetrabromobisphenol A and 2 mL n-hexyl Alkanes, mixed evenly, enriched with activated Li-SI small column, eluted with 1.4mL methanol, fixed to 1.5mL, filtered with 0.2μm PTFE filter (U.S. Pull company)...
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The invention provides a pretreatment method applied to analysis of tetrabromobisphenol A in biologically poisoned excrement, relates to detection analysis technology of organic pollutants in biologic samples, and can provide pretreatment technology for the determination of the content of the tetrabromobisphenol A in a biologically exposed and poisoned excrement sample. The pretreatment method comprises the following steps of freezing and drying the biologically exposed and poisoned excrement sample, adding methyl tertiary butyl ether and normal hexane solvent which are mixed in constant volume, carrying out ultrasonic extraction for three times by an ultrasonic cleaner, taking out the certain amount of extracting solution to be diluted, and then carrying out enrichment and purification on the diluted solution by an Li-SI solid-phase extraction cartridge. The pretreated sample is determined by an ultra-high performance liquid chromatography-tandem mass spectrometer, so that the pretreatment method applied to the analysis of the tetrabromobisphenol A in the biologically poisoned excrement has the advantages that the purification effect is good, the operations are simple, and the recovery rate is relatively high; the matrix interference is reduced by a diluting method, so that the pretreatment method is especially suitable for a pretreatment process of determination on the content of the tetrabromobisphenol A in the biologically exposed and poisoned excrement.
Description
technical field [0001] The invention relates to a detection and analysis technology for organic pollutants in biological samples, in particular to a sample extraction and purification method for analyzing the content of tetrabromobisphenol A in feces samples obtained after biological exposure and poisoning. Background technique [0002] In recent years, Tetrabromobisphenol A, as one of the brominated flame retardants with huge usage, has been widely used in household appliances and daily necessities, such as computers, printers, mobile phones, televisions, washing machines and other electronic products as well as textiles and foam furniture. , Building materials, etc. According to the report of the European Brominated Science and Environmental Forum (BSEF), in addition to Jordan, Israel, the United States, Japan, etc., my country is also a major producer of tetrabromobisphenol A. Due to the continuous increase in the production scale of related products, the continuous incr...
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IPC IPC(8): G01N30/06G01N30/08
Inventor 于云江王琼孙朋向明灯付益伟
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI