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Method for fast identifying key quasi/anti-androgen interference poison in water sample

An anti-androgen and androgen technology, applied in the field of pretreatment and measurement, can solve the problems of high cost and difficulty in identifying key androgen interferents, and achieve the effects of low cost, fewer steps, and less consumption of reagents

Active Publication Date: 2014-01-22
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of difficult identification and high cost of key androgen disruptors in existing environmental water bodies, the present invention provides a rapid identification method for key pseudo / anti-androgen disruptors in water samples, which can be used for identification and identification of endocrine disrupting toxicants in environmental water samples. Toxicity source analysis

Method used

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  • Method for fast identifying key quasi/anti-androgen interference poison in water sample
  • Method for fast identifying key quasi/anti-androgen interference poison in water sample
  • Method for fast identifying key quasi/anti-androgen interference poison in water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Select representative typical androgen disruptors with different properties, and accurately prepare 2 kinds of phthalates (Di-n-butyl phthalate, Di-2-ethylhexyl phthalate, the concentration is 100ng / L), 10 kinds of pesticides (α -BHC,β-BHC,γ-BHC,δ-BHC,o,p'-DDE,p,p'-DDE,o,p'-DDD,o,p'-DDD,o,p'-DDT, p, p'-DDT, the concentration is 50ng / L), 3 kinds of alkylphenols (nonylphenol, octylphenol and bisphenol A, the concentration is 200ng / L) water sample 5L, the extraction column is used in order Activate with 10mL of n-hexane, 5mL of dichloromethane, 5mL of acetone and 10mL of distilled water, and vacuum-dry under negative pressure. Concentrate by connecting HLB solid-phase extraction columns in series at a rate of 4 mL / min. Then eluted with 16 mL of n-hexane and dichloromethane with a volume ratio of 1:1, controlled the flow rate at 2 mL / min, collected the eluate every 2 mL, blown to 0.1 mL in a gentle nitrogen flow, and measured it by GC-MSMS . The analysis conditions are a...

Embodiment 2

[0038] The water sample was prepared by the method in Example 1, filtered and enriched by HLB solid-phase extraction column at a speed of 4 mL / min, the column was vacuum-dried under negative pressure and then blown dry with nitrogen. Then use 10 mL of a mixed solution of n-hexane and dichloromethane with a volume ratio of 1:1 for elution, and then use 8 mL of a mixed solution of dichloromethane and acetone with a volume ratio of 1:1 for elution, and control the flow rate to 2 mL / min. Collect the eluate every 2mL, and blow it to 0.1mL in a gentle nitrogen flow, respectively, use GC-MSMS to determine the phthalates, and analyze the alkylphenol compounds by HPLC:

[0039] Polar compound-based HPLC (DVD / FLD)

[0040] Mobile phase: 0-5min, 80% methanol & 20% water; 5-11min, 100% methanol; flow rate: 1ml / min; column temperature: 30°C.

[0041] Detector: TBBPA: UVD detector, detection wavelength λ=210nm;

[0042] BPA: FLD detector, 0-5min, λ Ex =228nm,λ Em =315nm;

[0043] OP, N...

Embodiment 3

[0083] Accurately formulated with known target pollutants containing 2 kinds of phthalates (Di-n-butyl phthalate, Di-2-ethylhexyl phthalate, the concentration is 100ng / L), 10 kinds of pesticides (α-BHC, β-BHC, γ -BHC, δ-BHC, o,p'-DDE, p,p'-DDE, o,p'-DDD, o,p'-DDD, o,p'-DDT, p,p'-DDT, concentration 50ng / L), 3 kinds of alkylphenols (nonylphenol, octylphenol and bisphenol A, the concentration is 200ng / L) water sample 5L, through the HLB solid phase extraction at the speed of 5mL / min Column enrichment. The extraction column was activated with 5 mL of n-hexane, 5 mL of dichloromethane, 5 mL of methanol, 5 mL of acetone and 10 mL of distilled water before use. After enrichment, the extraction column was vacuum-dried under negative pressure to remove most of the moisture, and then blown dry with nitrogen. Then eluted with 10 mL of n-hexane and dichloromethane with a volume ratio of 1:1, and then eluted with 8 mL of dichloromethane and acetone with a submission ratio of 1:1. The flo...

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Abstract

The invention discloses a method for fast identifying key quasi / anti-androgen interference poison in a water sample. The method mainly comprises the following steps that enrichment is carried out on the water sample through solid-phase extraction columns, and negative-pressure hollow drying is carried out on the extraction columns; the extraction columns are eluted through organic solvents in sequence, concentration and volume measurement are carried out on eluent, one half of the eluent is used for the toxicity test of quasi / anti-androgens, the total toxic equivalent is calculated based on a standard substance EC50 and the dilution ratio, and the other half of the eluent is used for identifying the main toxic substances of a toxic sample; based on the spectrum signature and the toxic equivalent of common quasi / anti-androgen active poison, a poison mass balance database is built, then the toxic equivalent and the toxic contribution rate are calculated based on the results of qualitative analysis and quantitative analysis, and the main toxic substances are determined. According to the method, the number of demanded samples is small, reagent consumption is little, cost is low, the number of the steps is small, and the quasi / anti-androgen poison in water bodies with different pollution levels can be identified fast.

Description

technical field [0001] The invention relates to a pretreatment and determination method for rapid identification of pseudo / anti-androgen interference poisons in water bodies with different pollution degrees, more specifically, it is a method that combines chemical analysis and toxic equivalent calculation, which is aimed at containing common pseudo / androgen interference poisons. The complex environmental water samples of anti-androgen interference active substances are extracted with the same column, and then based on the mass balance database, the established toxic equivalent calculation method and the SRM scanning mode of GC-MSMS are used to quickly identify the source of toxicity for toxicant screening. Background technique [0002] With the development of the economy and the continuous improvement of people's living standards, a large number of organic pollutants are continuously discharged into the water body environment in the process of industrial and agricultural prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 史薇于红霞王小享胡欣欣王玉婷
Owner NANJING UNIV
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