A pretreatment method for the analysis of tetrabromobisphenol A in biological urine
A technology of tetrabromobisphenol and urine is applied in the field of detection and analysis of organic pollutants in biological samples, which can solve problems such as persistent organic pollution, and achieve the effects of high recovery rate, accurate determination and good impurity removal effect.
Inactive Publication Date: 2016-04-20
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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Problems solved by technology
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 urine
[0027] Accurately pipette the urine, add 10ngC13-labeled tetrabromobisphenol A, adjust the pH value of the urine sample to 5.5 with 6moL / L hydrochloric acid, add 0.5mL sodium acetate buffer solution with a pH value of 5.5 and 10μL β-glucuronide / aryl sulfate For lipase, place in a constant temperature shaker in a water bath at 37°C and avoid light for 4 hours; add a small amount of methanol to the hydrolyzed solution and mix evenly, enrich with an activated ENVI-18 column, rinse with 3mL of 5% methanol water, and rinse with 2mL of two Elute with methyl chloride and 3 mL of methanol; after mixing the eluent evenly, add 10 mL of 1% hydrochloric acid solution and 10 mL of dichloromethane solvent, vortex and oscillate to mix evenly, place in a centrifuge and centrifuge at 3000 rpm for 5 minutes, recover Dich...
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The invention discloses a pretreatment method for analyzing tetrabromobisphenol A in biologic urine, relates to a detection and analysis technique of organic pollutant in a biologic sample, and provides a pretreatment technique for testing the content of tetrabromobisphenol A in urine. The pretreatment method comprises the following steps: regulating the pH value in a urine sample, performing enzymolysis on the urine in a mode of adding beta-glucuronide / aryl sulfuric acid lipase, enriching enzymatic hydrolysate through an ENVI-18 column, washing the enriched eluant by using a 1% hydrochloric acid solution and dichloromethane in a vortex and shaking manner, and subsequently washing a recycled organic layer by using distilled water for another time. The detection on the sample by using an ultra-high performance liquid chromatography-tandem mass spectrometer shows that the method is simple to operate, high in recycling rate and good in impurity moving effect, is applicable to pretreatment on the biologic urine sample, and is particularly applicable to extraction and purification operation on a large-scale biologic urine sample. By adopting the method, conjugate of the tetrabromobisphenol A in the sample can be effectively decomposed, the urine sample can be effectively purified, and support is provided for detection on the tetrabromobisphenol A in the urine.
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 biological urine. 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 (BrominatedScienceandEnvironmentalForum, 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 increase i...
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IPC IPC(8): G01N30/06G01N30/88
Inventor 于云江王琼孙朋向明灯张艳平
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI