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Method for measuring phenolic estrogen by means of derivation

A phenolic estrogen and derivatization technology, which is applied in the field of veterinary drug residue analysis and detection, can solve the problems of low sensitivity, low ionization efficiency, and short start-up vacuum time, etc., and achieves improved sensitivity, low detection cost, and good reproducibility Effect

Inactive Publication Date: 2016-08-10
INST OF QUALITY STANDARD & DETECTION TECH YUNNAN ACAD OF AGRI SCI
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Problems solved by technology

At present, the UPLC system is equipped with a portable mass spectrometer detector (QDa), which has better sensitivity and accuracy than the ultraviolet detector (PDA). It is ready to use and is suitable for daily detection of large quantities of samples. However, it also has the disadvantages of low ionization efficiency and low sensitivity for estradiol and estrol compounds. Require

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  • Method for measuring phenolic estrogen by means of derivation
  • Method for measuring phenolic estrogen by means of derivation
  • Method for measuring phenolic estrogen by means of derivation

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Experimental program
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Effect test

Embodiment 1

[0053] Embodiment 1 Derivatization reaction conditions

[0054] ① Preparation of dansyl chloride derivatization reagent: Dissolve solid dansyl chloride in acetone solvent to prepare a dansyl chloride derivatization reagent with a concentration of 1 mg / mL, put it into a brown bottle, and store it in a -20°C refrigerator.

[0055] ② Derivatization reaction condition 1: Add 10 μL of 1 mg / mL dansyl chloride derivatization reagent prepared in step (1) ①, adjust the pH of the mixture to 8.0 with sodium bicarbonate, vortex mix for 30 seconds, and derivatize at 45°C for 10 minutes .

[0056] ③ Derivatization reaction condition 2: Add 100 μL of 1 mg / mL dansyl chloride derivatization reagent prepared in step (1) ①, adjust the pH of the mixture to 9.0 with sodium bicarbonate, vortex mix for 30 seconds, and derivatize at a temperature of 55°C for 10 minutes .

[0057] ④ Derivatization reaction condition 3: Add 200 μL of the 1 mg / mL dansyl chloride derivatization reagent prepared in step...

Embodiment 2

[0060] The preparation of embodiment 2 estrogen standard samples and estrogen standard curve drawing

[0061] (1) Preparation of estrogen standard samples

[0062] ①Preparation of standard stock solution: Dissolve the following six estrogen solid standards: 17β-estradiol, estriol, estrone, diethylstilbestrol, hexestrol, and diethylstilbestrol, respectively, in methanol to prepare The following 6 standard stock solutions with a concentration of 1mg / mL:

[0063] 1mg / mL 17β-estradiol standard stock solution;

[0064] 1mg / mL estriol standard stock solution;

[0065] 1mg / mL estrone standard stock solution;

[0066] 1mg / mL diethylstilbestrol standard stock solution;

[0067] 1mg / mL standard stock solution of hexestrol;

[0068] Dienestrol standard stock solution of 1mg / mL;

[0069] The above six standard stock solutions were stored in a -20°C refrigerator.

[0070] ②Preparation of five serial concentrations of mixed standard solutions: measuring step (1) ① The prepared concen...

Embodiment 3

[0095] Example 3 milk sample detection

[0096] (1) Extraction of milk samples

[0097] The market randomly selects milk as the experimental sample, and simultaneously detects the above six estrogen residues. A total of 3 added concentrations were set, which were 2, 10, and 50 μg / kg. A blank sample was set up, each concentration was repeated 6 times, and the repeatability experiment was carried out, and the recovery rate and variation coefficient were calculated respectively.

[0098] (2) Derivatization reaction

[0099] Accurately weigh 5 g of sample, add 100 μL of the internal standard with a concentration of 500 ng / mL prepared in step (1) ③ of Example 2, collect the eluate after extraction and purification, blow dry with nitrogen, add a volume of 200 μL in step (1) of Example 2 ) ④ prepare 1mg / mL dansyl chloride derivatization reagent, adjust the pH to 10 with sodium bicarbonate, vortex mix for 30s, and react at 60°C for 30min to obtain the derivatized product. Take it ...

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Abstract

The invention discloses a method for measuring phenolic estrogen by means of derivation. The method includes simultaneously deriving six types of phenolic estrogen; quickly measuring the phenolic estrogen by the aid of ultrahigh-performance liquid chromatography-mass spectrometry detectors. Compared with the prior art, the method has the advantages that the sensitivity of the six types of phenolic estrogen can be improved, the method is good in repeatability and low in detection cost and only has small variable coefficients, and measurement requirements on recovery rates can be met.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection of veterinary drug residues, and uses an ultra-high performance liquid chromatography-mass spectrometer to simultaneously measure estradiol and estrone through a pre-column derivatization reaction. The invention can simultaneously analyze and measure multi-residue estrogen and estrogen estrogen in animal tissues, and can also analyze and measure other polyphenolic organic substances. Background technique [0002] Estrogen is a class of steroid compounds with a wide range of biological activities, which can promote and maintain female-related physiological functions, and also exert special effects on the endocrine system, cardiovascular system, body metabolism, bone development and skin. Natural steroid hormones are mainly produced by the female or male sex organs of animals, adrenaline and other organs, and are one of the important substances for animal growth and development, such ...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 刘宏程黎其万林涛李宁邵金良汪禄祥
Owner INST OF QUALITY STANDARD & DETECTION TECH YUNNAN ACAD OF AGRI SCI
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