Method for detecting trace phenols environmental estrogen

A technology of environmental estrogen and phenols, applied in the field of biological samples and environmental inspection (monitoring), can solve the problems of cumbersome operation process, pollution, high detection cost, etc., achieve high enrichment multiple, high enrichment efficiency, and easy operation Effect

Inactive Publication Date: 2014-02-05
WENZHOU MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most of the existing extraction technologies still rely on liquid-liquid extraction or solid-phase extraction for separation and enrichment. The operation process is relatively cumbersome, the organic

Method used

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  • Method for detecting trace phenols environmental estrogen
  • Method for detecting trace phenols environmental estrogen
  • Method for detecting trace phenols environmental estrogen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Detection of phenolic environmental estrogens in tap water:

[0032] Take 15mL of tap water and pass through a 0.22μm filter membrane; take 10mL of filtered tap water in a 15mL centrifuge tube, add 0.3mL of concentrated sulfuric acid to adjust the pH of the solution to 3, then add 500μL of SDS and 50μL of CHCl 3 , Shake the mixture well, and ultrasonically mix, the ultrasonic power is 400W, the switching interval is 5s:3s, a total of 50 times, centrifuge at 5000rpm for 2min, and small droplets are formed at the bottom; use a micro sampler to absorb small droplets at the bottom 40 μL, using the optimized high performance liquid chromatography conditions to quantitatively detect the content of phenolic environmental estrogens, the mobile phase is acetonitrile and deionized water, the gradient elution conditions are: 0~6min, acetonitrile:water=45:55; 6~20min , acetonitrile:water=70:30; the column temperature is 25°C, the ultraviolet wavelength is 270nm, the flow rate is 0....

Embodiment 2

[0034] Detection of phenolic environmental estrogens in Spirulina-350 (ASP-350):

[0035] Take 10mL water sample of Spirulina ASP-350 in the logarithmic growth phase, put it in a 15mL centrifuge tube, add deionized water to 15mL, centrifuge for 2min, remove the supernatant; add deionized water to the ASP-350 precipitated at the bottom of the tube to 10mL, centrifuge for 2min, then add water to the precipitated ASP-350 cells to 10mL; ultrasonically break, the power is 400W, the on-off interval is 5s:3s, the number of on-off intervals is 50 times, and the total crushing treatment time is 400s; add 0.3mL of concentrated sulfuric acid Place in the centrifuge tube for 2 minutes, centrifuge at 5000 rpm for 2 minutes; take the supernatant to adjust the pH to 3, add 500 μL of surfactant SDS and 50 μL of extractant CHCl 3 , ultrasonic mixing, ultrasonic power 400W, switching interval 5s:3s, a total of 50 times, high-speed low-temperature centrifugation, rotation speed 5000rpm, temperat...

Embodiment 3

[0037] Detection of phenolic environmental estrogens in Spirulina-834 (ASP-834):

[0038] Take 10mL water sample of Spirulina ASP-834 in the logarithmic growth phase, put it in a 15mL centrifuge tube, add deionized water to 15mL, centrifuge for 2min, remove the supernatant; add deionized water to the ASP-834 precipitated at the bottom of the tube to 10mL, centrifuge for 2min, then add water to the precipitated ASP-834 cells to 10mL; ultrasonically break, the power is 400W, the on-off interval is 5s:3s, the number of on-off intervals is 50 times, and the total crushing treatment time is 400s; add 0.3mL of concentrated sulfuric acid Place in the centrifuge tube for 2 minutes, centrifuge at 5000 rpm for 2 minutes; take the supernatant to adjust the pH to 3, add 500 μL of surfactant SDS and 50 μL of extractant CHCl 3 , ultrasonic mixing, ultrasonic power 400W, switching interval 5s:3s, a total of 50 times, high-speed low-temperature centrifugation, rotation speed 5000rpm, temperatur...

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Abstract

The invention discloses a method for detecting trace phenols environmental estrogen and belongs to the technical field of biological samples and environment detection (monitoring). According to the method, the extraction comprises the following steps: adjusting the pH (Potential of Hydrogen) value of a solution to be detected to be 2.5-3.5; adding a surfactant and an extracting agent; uniformly mixing by ultrasonic waves; centrifuging at a low temperature; removing an upper layer; quantitatively detecting by adopting a high performance liquid chromatography. According to the method, an ultrasonic wave assisting surfactant emulsification and micro-extraction technology is adopted and the surfactant with low toxin is used for replacing toxic dispersants including acetone, methanol, acetonitrile and the like; the high performance liquid chromatography (HPLC) is combined to be used for quantitative detection; the method has the advantages of high efficiency, low toxin, simplicity and convenience in operation, low cost and the like; the enriching multiple is up to more than 200 times and the detection range is within 0.01 microgram/liter-0.1 microgram/liter; the method can be widely applied to detecting (monitoring) and analyzing the phenols environmental estrogen in spiral seaweed biological samples, foods and medicines.

Description

technical field [0001] The invention specifically relates to a method for detecting trace amounts of phenolic environmental estrogen, and belongs to the technical field of biological samples and environmental inspection (monitoring). Background technique [0002] Phenolic environmental estrogens are the most common class of pollutants with estrogenic activity in the environment. A large number of environmental survey results and laboratory studies have shown that phenolic environmental estrogens such as bisphenol A, pentachlorophenol and estradiol have a significant effect on the increase in the incidence of male testicular and prostate cancer, the decrease in sperm count, female breast cancer, Increased incidence of uterine cancer, feminization of male animals, and changes in immune function all play a role that cannot be ignored. Therefore, phenolic environmental estrogens (PEs) have become a hot spot pollutant in research and monitoring in recent years. At present, coun...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14G01N30/06
Inventor 王慧利王学东王永魁
Owner WENZHOU MEDICAL UNIV
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