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Method for rapidly measuring natural estrogen combination

A rapid determination and estrogen technology, applied in the field of analysis and detection, can solve the problems of low reagent cost, high cost, long time consumption, etc., and achieve the effect of simple operation, low cost and wide application prospect.

Inactive Publication Date: 2019-04-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the deconjugation of natural estrogen conjugates is mainly based on the enzymatic hydrolysis method, but the enzymatic hydrolysis method has the disadvantages of high cost and a reaction time of up to 24 hours
In the early stage, the application team established a method for rapid removal of natural estrogen conjugates by acid solvent solution. Not only the cost of reagents is low, but the reaction time only takes 2 hours, but the reaction solution after the removal of conjugates still needs to be further concentrated, which is time-consuming. long

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  • Method for rapidly measuring natural estrogen combination
  • Method for rapidly measuring natural estrogen combination
  • Method for rapidly measuring natural estrogen combination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 50 μL of methylformamide solution to the test tubes containing natural estrogen sulfate conjugates E1-3S, E2-3S, and E3-3S, mix thoroughly, and then add 50 mL of BSTFA (containing 1% TMCS). Tighten the glass test tube with the cap. Then put the glass test tube into an oven and react at 80°C for 90 minutes. After cooling, blow off with a slow nitrogen flow. After the solution is completely dried, add 900 μL of ethyl acetate, mix and dissolve thoroughly, and then use a pipette gun to transfer the resulting solution to a 2 mL sample injection bottle for GC-MS Analysis and analysis of the measurement results are shown in Table 1.

[0018] Table 1 Determination results of natural estrogen sulfate conjugates

[0019] Natural Estrogen Sulfate Conjugate

[0020]

Embodiment 2

[0022] Add 50 μL of ethyl acetate organic solution to the test tubes containing natural estrogen sulfate conjugates E1-3S, E2-3S, and E3-3S, mix thoroughly, and then add 50 mL of BSTFA (containing 1% TMCS). Tighten the glass test tube with the cap. Then put the glass test tube into an oven and react at 80°C for 120 minutes. After cooling, blow off with a slow nitrogen flow. After the solution is completely dried, add 900 μL of ethyl acetate, mix and dissolve thoroughly, and then use a pipette gun to transfer the resulting solution to a 2 mL sample injection bottle for GC-MS Analysis, measurement result analysis is shown in Table 2. Please refer to Example 1 for the determination accuracy formula.

[0023] Table 2 Determination results of natural estrogen sulfate conjugates

[0024] Natural Estrogen Sulfate Conjugate

Embodiment 3

[0026] Add 50 μL of ethyl acetate organic solution to the test tubes containing natural estrogen sulfate conjugates E1-3S, E2-3S, and E3-3S, mix thoroughly, and then add 50 mL of BSTFA (containing 1% TMCS). Tighten the glass test tube with the cap. Then put the glass test tube into an oven and react at 80°C for 150 minutes. After cooling, blow off with a slow nitrogen flow. After the solution is completely dried, add 900 μL of ethyl acetate, mix and dissolve thoroughly, and then use a pipette gun to transfer the resulting solution to a 2 mL sample injection bottle for GC-MS Analysis, measurement result analysis is shown in Table 3. Please refer to Example 1 for the determination accuracy formula.

[0027] Table 3 Determination results of natural estrogen sulfate conjugates

[0028] Natural Estrogen Sulfate Conjugate

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Abstract

The invention belongs to the technical field of analysis and detection, and discloses a method for rapidly measuring a natural estrogen combination. A sulfuric acid combination sample containing a natural estrogen is enriched by a solid-phase extraction column and then is added into an organic solvent to be uniformly mixed, then a derivatization reagent BSTFA is added, and derivatization reactionis carried out at the temperature of 60-90 DEG C; and an organic solvent is removed after the reaction is completed, and a reaction product is dissolved by using ethyl acetate to carry out GC-MS analysis. Compared with a conventional analysis method, the method has the greatest characteristic that decombination and sample re-concentration process which are complicated in operation are omitted, andhas the advantages of being easy to operate, low in cost, rapid and the like, and has a wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a method for quickly measuring natural estrogen conjugates. Background technique [0002] Natural estrogen is a general term for a class of steroid compounds. There are as many as 17 known natural estrogens, mainly including estrone (estrone, E1), estradiol (17β-estradiol, E2) and estriol (estriol, E3). The basic functions of natural estrogens are Maintain the normal operation of the endocrine function of the human body and animals. In the past two decades, natural estrogens, as a class of environmental interfering chemicals, have received worldwide attention. In the latest Japanese drinking water quality standards, estradiol has been listed as a temporary water quality indicator. The natural estrogen in the environment mainly comes from the excretion of human body and animals, and is mainly excreted with urine. Natural estrogen in urine exists in t...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 刘则华尹华党志
Owner SOUTH CHINA UNIV OF TECH