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Derivatization method of environmental estrogens

An environmental estrogen and derivatization technology, applied in the field of derivatization of environmental estrogen, can solve the problems of increasing energy consumption and cost of derivatization experiments, reducing detection accuracy, increasing sample loss, etc., and simplifying the derivatization reaction system. , The effect of reducing the experimental cost and reducing the loss of samples

Inactive Publication Date: 2010-04-21
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In short, the disadvantages of the current derivatization method of environmental estrogen are: the derivatization reaction needs to be carried out under heating conditions, the heating temperature is 60-80°C, the heating time is 30min-15h, and a catalyst needs to be added, which makes the derivatization The energy consumption and cost of the experiment increase, the operation steps are cumbersome, and the experiment time is longer. In the actual environmental sample detection, the sample loss is increased and the detection accuracy is reduced.

Method used

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  • Derivatization method of environmental estrogens
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  • Derivatization method of environmental estrogens

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. First, take 100 μL of the standard mixed solution containing a certain concentration (10pg / μL) of E1, E2, EE2, and E3 in a 1.5mL chromatographic bottle, put the chromatographic bottle into a nitrogen blower, and blow it dry slowly with high-purity nitrogen.

[0039] 2. Add 15 μL of BSTFA and 30 μL of pyridine, shake and mix, and place in a normal temperature environment (20° C.) for 3 minutes to react.

[0040] 3. Take it out and cool it to room temperature, put it into a nitrogen blower, blow it dry slowly with high-purity nitrogen, add 90 μL of injection solvent and 10 μL of internal standard (androstane) with a concentration of 1 ng / μL, shake and mix, take 1 μL and inject GC-MS analysis (SIM mode).

[0041] After testing, E1, E2, EE2, and E3 have all been derivatized, and the derivatized products are TMS-E1, di-TMS-E2, di-TMS-EE2, tri-TMS-E3, no by-products are generated, RRF( The relative response factor RelativeResponse Factor, the ratio of the peak area of ​​t...

Embodiment 2

[0043] 1. First, take 100 μL of the standard mixed solution containing a certain concentration (10ng / μL) of E1, E2, EE2, and E3 in a 1.5mL chromatographic bottle, put the chromatographic bottle into a nitrogen blower, and blow it dry slowly with high-purity nitrogen.

[0044] 2. Add 30 μL of BSTFA and 50 μL of pyridine, shake and mix, and place in a room temperature environment (20° C.) to react for 5 minutes.

[0045] 3. Take it out and cool it to room temperature, put it into a nitrogen blower, blow it dry slowly with high-purity nitrogen, add 90 μL of injection solvent and 10 μL of internal standard (androstane) with a concentration of 1 ng / μL, shake and mix, take 1 μL and inject GC-MS analysis (SIM mode).

[0046] After testing, E1, E2, EE2, and E3 have all been derivatized, and the derivatized products are TMS-E1, di-TMS-E2, di-TMS-EE2, tri-TMS-E3, respectively, and no by-products are generated. For 1157.76, 1074.82, 146.65, 187.13.

Embodiment 3

[0048] 1. First, take 100 μL of the standard mixed solution containing a certain concentration (8pg / μL) of E1, E2, EE2, and E3 in a 1.5mL chromatographic bottle, put the chromatographic bottle into a nitrogen blower, and blow it dry slowly with high-purity nitrogen.

[0049] 2. Add 15 μL of BSTFA and 20 μL of pyridine, shake and mix, put into a constant temperature heating box, and react at 30°C for 3 minutes.

[0050] 3. Take it out and cool it to room temperature, put it into a nitrogen blower, blow it dry slowly with high-purity nitrogen, add 90 μL of injection solvent and 10 μL of internal standard (androstane) with a concentration of 1 ng / μL, shake and mix, take 1 μL and inject GC-MS analysis (SIM mode).

[0051] After testing, E1, E2, EE2, and E3 have all been derivatized, and the derivatized products are TMS-E1, di-TMS-E2, di-TMS-EE2, tri-TMS-E3, respectively, and no by-products are generated. 0.99, 0.88, 0.06, 0.08.

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Abstract

The invention discloses a derivatization method of environmental estrogens (estrone, 17beta-estradiol, estriol, 17alpha-ethynylestradiol), which is a treatment method and a core technology before a gas chromatography-mass spectrum (GC-MS) is used for analyzing the samples of the substances. The method comprises the following steps: firstly, leading high-purity nitrogen in at a room temperature to dry a standard mixed solution containing environmental estrogens; adding derivative reagents N, O-BSTFA and pyridine to react at room temperature (20 DEG C)-50 DEG C to obtain derivative products; drying; adding a sampling solvent and an internal standard; sampling and analyzing. The method has the advantages of simple and convenient experimental operation, time saving and low energy consumption and cost, simultaneously derivates the four environmental estrogens without generating side products, has favorable linear correlation among various derivative products and achieves an instrument detection limit up to 0.5pg / muL, thereby being applied to the GC-MS detection of environmental estrogens in water bodies, sediment, biological samples, and the like.

Description

technical field [0001] The invention belongs to the field of environmental analytical chemistry, relates to a derivatization method of environmental estrogen (estrone, 17β-estradiol, estriol, 17α-ethinyl estradiol), and is used for gas chromatography-mass spectrometry Sample pretreatment methods and core technologies for the analysis of such substances. Background technique [0002] Environmental hormones (Environmental Hormones) refer to the exogenous chemical substances existing in the environment that can interfere with various aspects of the endocrine system of humans or wild animals and affect the functions of reproductive, nervous and immune systems. Environmental hormones are highly toxic and bioaccumulative, and can interfere with the endocrine system of animals and humans through drinking water and food chain enrichment. At extremely low concentrations (ng / L level), they can cause serious harm to organisms, not only affecting Human health and continued reproduction...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/72
Inventor 潘学军黄斌刘晶靓方锴王宇高建培
Owner KUNMING UNIV OF SCI & TECH
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