Method for detecting and analyzing multiple EDCs (endocrine disruptor chemicals) in environments and food

A technology of endocrine disruptors and analysis methods, which is applied in the direction of analysis materials, measuring devices, material separation, etc., can solve the problems of low concentration of endocrine disruptors, high derivatization reaction temperature, easy hydrolysis of derivatization reagents, etc., to achieve stable derivative products and improve Chromatographic resolution and detection sensitivity, the effect of improving method sensitivity

Active Publication Date: 2016-10-12
食药环检验研究院(山东)集团有限公司
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Problems solved by technology

[0003] However, the concentration of various endocrine disruptors in the environment and food is extremely low, usually ng / L or even pg / L, and they are greatly disturbed by the complex matrix of the environment. Therefore, it is necessary to establish fast and efficient environmental and food pretreatment technologies and instruments Analytical methods are necessary
Chinese patent (CN102043028A) discloses a method of using N, O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and pyridine as derivatization reagents to derivatize estrone and 17β-estrone by gas chromatography-mass spectrometry. The analysis and detection method of diol, diethylstilbestrol, nonylphenol, and octylphenol has a long derivation time, and the derivatization reagent is easy to hydrolyze, and the sensitivity is low; Chinese patent (CN103185762A) utilizes dansyl chloride to derive estrone and 17β-estradiol in food Alcohol, diethylstilbestrol, octylphenol, but the derivation reaction temperature of this method is high, the time is long, and the reagent itself and the derivative product are easy to decompose

Method used

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  • Method for detecting and analyzing multiple EDCs (endocrine disruptor chemicals) in environments and food
  • Method for detecting and analyzing multiple EDCs (endocrine disruptor chemicals) in environments and food
  • Method for detecting and analyzing multiple EDCs (endocrine disruptor chemicals) in environments and food

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Embodiment 1

[0038] Chromatographic separation and qualitative and quantitative analysis of 23 endocrine disruptors and 3 internal standards:

[0039] 23 kinds of endocrine disruptors and 3 kinds of internal standards (purchased from Sigma and Aladdin Reagent Company) were prepared in acetonitrile to obtain a concentration of 1.0 × 10 -5 mol / L standard solution of endocrine disruptors, take 0.2 mL from each single standard stock solution and dilute to 10 mL to obtain a mixed standard stock solution of endocrine disruptors. 4'-Carbonyl chloride-rhodamine was dissolved in acetonitrile to give 1.0 × 10 -2 mol / L derivatization reagent acetonitrile solution; take 70 µL of the standard solution and place it in a 1.5 mL centrifuge tube, add 30 µL of the internal standard solution (the internal standard solution is 10 µL with a concentration of 1×10 -5 mol / L estrone-2,4,16,16-d 4 , 10 µL concentration is 1×10 -5 mol / L Bisphenol A-d 16 , 10 µL concentration is 1×10 -5 mol / L methyl-4-hydro...

Embodiment 2

[0044] The detection and analysis of endocrine disruptors in domestic wastewater includes the following steps:

[0045] Take 1000 µL of domestic wastewater and filter it with a 0.45 µm water filter membrane, add HCl to adjust the pH to 6.0, then take 100 µL of water sample and place it in a 1.5 mL centrifuge tube, add 30 µL of internal standard solution (10 µL concentration is 1×10 -5 mol / L estrone-2,4,16,16-d 4 , 10 µL concentration is 1×10 -5 mol / L Bisphenol A-d 16 , 10 µL concentration is 1×10 -5 mol / L methyl-4-hydroxybenzoate-2,3,5,6-d 4 ), add 800 µL NaHCO 3 -Na 2 CO 3 (pH 11.5) buffer solution, and quickly inject 200 µL bromobenzene and 300 µL molar concentration of 1×10 -2 mol / L 4'-carbonyl chloride-rhodamine-acetonitrile solution, vortex mixer for 5 s to mix the solution evenly. After ultrasonic oscillation at 25 ºC for 1 min, centrifuge at high speed for 2 min at 12000 r / min. The organic phase was deposited at the bottom of the centrifuge tube, and the dep...

Embodiment 3

[0047] The detection of endocrine disruptors in river sediments includes the following steps:

[0048] references( Journal of Chromatography A , 2013, 1305: 17–26), take 0.8 g of river sediment samples and place them in a 20 mL centrifuge tube, add 3 mL of methanol, perform ultrasonic extraction for 30 min, centrifuge for 10 min, filter, and transfer the supernatant to a vial , as mentioned above, the residue was extracted again; the supernatant was combined and rotary evaporated to about 1 mL, and the volume was adjusted to 10 mL with ultrapure water, and 90 µL was placed in a 1.5 mL centrifuge tube, and 30 µL of the internal standard solution ( 10 µL concentration is 1×10 -5 mol / L estrone-2,4,16,16-d 4 , 10 µL concentration is 1×10 -5 mol / L Bisphenol A-d 16 , 10 µL concentration is 1×10 -5 mol / L methyl-4-hydroxybenzoate-2,3,5,6-d 4 ), add 900 µL of NaHCO pH 8.0 3 -Na 2 CO 3 buffer solution, and quickly injected with 120 µL 1-bromo-3-methylbutane and 200 µL molar...

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Abstract

The invention belongs to the technical field of analysis chemistry and particularly relates to a method for detecting and analyzing multiple EDCs (endocrine disruptor chemicals) in the environments and food. According to the detection and analysis method, 4'-phosgene-rhodamine is taken as a derivatization reagent, and the multiple EDCs are analyzed through ultrasonic-assisting-in-situ derivatization-dispersive liquid-liquid microextraction in combination with ultra-high performance liquid chromatography triple quadrupole mass spectrometry detection. According to the method, 4'-phosgene-rhodamine containing an intramolecular permanent positive charge is taken as the derivatization reagent for the first time, 23 EDCs are measured, and quantitation is performed with a tandem mass spectrometry multi-reaction monitoring mode in combination with an internal standard method. The method is environment-friendly, simple, rapid, high in sensitivity and good in selectivity, the recovery rate is good, and matrix interference of actual samples is effectively reduced. The method is applicable to detection and analysis of the EDCs in various environments and food samples, and an accurate and reliable technical means is provided for monitoring and evaluation of the environments and the food.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for detecting and analyzing various endocrine disruptors in the environment and food, in particular to a method of using 4'-carbonyl chloride-rhodamine as a derivatizing reagent, ultrasonic-assisted-in-situ derivatization - A method for the analysis of various endocrine disruptors by dispersive liquid-liquid microextraction combined with ultra-high performance liquid chromatography triple quadrupole mass spectrometry detection. Background technique [0002] Endocrine disruptor chemicals (EDCs), also known as environmental estrogen, is a class of exogenous interfering substances that can simulate and interfere with the normal synthesis, transportation, and binding of estrogen in humans or animals, mainly including Existing estrone (E1), 17β-estradiol (E2), estriol (E3), and synthetic 17α-ethinyl estradiol (EE2), diethylstilbestrol (DES), alkylphen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062G01N2030/067
Inventor 赵先恩魏娜王仁君颜平王玉花和永瑞宋翠华朱树芸尤进茂
Owner 食药环检验研究院(山东)集团有限公司
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