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Hydroxyl group/keto group synchronous derivatization method of steroid environment endocrine disturbing chemicals

A technology based on endocrine disruptors and hydroxyketones, which is applied in the field of environmental analytical chemistry, can solve the problems of large differences in catalyst addition, reduced detection accuracy, increased energy consumption and cost, and saves heating steps and reduces experimental costs. , the effect of reducing energy consumption and cost

Inactive Publication Date: 2011-01-12
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The derivatization reaction needs to be carried out under heating conditions. The heating temperature is 60-80°C, the heating time is 15min-1h, and the amount of catalyst added varies greatly. This will increase the energy consumption and cost of the derivatization experiment, and the experiment time will be longer. In the actual environmental sample detection, the sample loss is increased and the detection accuracy is reduced

Method used

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  • Hydroxyl group/keto group synchronous derivatization method of steroid environment endocrine disturbing chemicals
  • Hydroxyl group/keto group synchronous derivatization method of steroid environment endocrine disturbing chemicals
  • Hydroxyl group/keto group synchronous derivatization method of steroid environment endocrine disturbing chemicals

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The concrete steps of hydroxyketone synchronous derivatization method are:

[0036] 1. First, accurately weigh 10 mg of E1, E2, EE2, E3, PROG, and internal standard into 10 mL chromatographic bottles, respectively add 10 mL of methanol, shake for 60 s, and prepare standard stock solutions with a concentration of 1 μg / μL, seal Store at -20°C for later use; use methanol and standard stock solution to prepare a standard mixed solution containing E1, E2, EE2, E3, PROG at a concentration of 5pg / L and an internal standard at a concentration of 100pg / μL;

[0037] 2. Take 100 μL of the standard mixed solution prepared in step (1) in a 1.5 mL chromatographic bottle, put the chromatographic bottle into a nitrogen blower, and blow dry slowly with nitrogen gas with a purity of 99.99%;

[0038] 3. Add 100 μL of MSTFA / TMIS / DTE (1000:5:5, v / v / w), shake for 30 seconds to mix, and place in a dry and heated environment at 20°C for 10 minutes to react;

[0039] 4. Take out and cool to ro...

Embodiment 2

[0042] The concrete steps of hydroxyketone synchronous derivatization method are:

[0043] 1. First, accurately weigh 10 mg of E1, E2, EE2, E3, PROG, and internal standard into 10 mL chromatographic bottles, respectively add 10 mL of methanol, shake for 60 s, and prepare standard stock solutions with a concentration of 1 μg / μL, seal Store at -30°C for later use; use methanol and standard stock solution to prepare a standard mixed solution containing E1, E2, EE2, E3, PROG at a concentration of 5pg / L and an internal standard at a concentration of 100pg / μL;

[0044] 2. Take 100 μL of the standard mixed solution prepared in step (1) in a 1.5 mL chromatographic bottle, put the chromatographic bottle into a nitrogen blower, and blow dry slowly with nitrogen gas with a purity of 99.99%;

[0045] 3. Add 100 μL of MSTFA / TMIS / DTE (1000:5:5, v / v / w), shake for 30 seconds to mix, and place in a dry and heated environment at 20°C for 5 minutes to react;

[0046] 4. Take out and cool to roo...

Embodiment 3

[0049] The concrete steps of hydroxyketone synchronous derivatization method are:

[0050] 1. First, accurately weigh 10 mg of E1, E2, EE2, E3, PROG, and internal standard into 10 mL chromatographic bottles, respectively add 10 mL of methanol, shake for 60 s, and prepare standard stock solutions with a concentration of 1 μg / μL, seal Store at -40°C for later use; use methanol and standard stock solution to prepare a standard mixed solution containing E1, E2, EE2, E3, PROG at a concentration of 5pg / L and an internal standard at a concentration of 100pg / μL;

[0051] 2. Take 100 μL of the standard mixed solution prepared in step (1) in a 1.5 mL chromatographic bottle, put the chromatographic bottle into a nitrogen blower, and blow dry slowly with nitrogen gas with a purity of 99.99%;

[0052] 3. Add 100 μL of MSTFA / TMIS / DTE (1000:5:5, v / v / w), shake for 30 seconds to mix, then place in a dry and heated environment at 30°C for 7 minutes to react;

[0053] 4. Take out and cool to ro...

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Abstract

The invention discloses a steroid environment endocrine disturbing chemicals hydroxyl group / keto group synchronous derivatization method of steroid environment endocrine disturbing chemicals (oestrone, 17 beta-estradiol, 17 alpha-ethinyl estradiol, estriol and progesterone). The method comprises the following steps: first fetching standard mixed solution containing the steroid environment endocrine disturbing chemicals and internal standard and introducing high-purity nitrogen at normal temperature so as to dry the standard mixed solution; and adding derivatization reagent prepared from N-methyl-N-trimethylsilyl trifluoroacetamide, iodotrimethylsilane and dithiothreitol based on a proportion of 1,000 muL:5 to 10 muL:5 mg and reacting at 20 to 60 DEG C for 5 to 10 min so as to obtain the derivatization product shown in figure. The method has the advantages of simple and time-saving operation, low energy consumption and cost and the like. The hydroxyl group and the keto group can be derivatized synchronously, the linear correlation among the derivatization products is good, and the detection limit of instrument can reach 0.01 to 1 pg / mu L. The method can be used for the GC-MS detection of the steroid environment endocrine disturbing chemicals in samples such as water, bottom sediment, organisms and the like.

Description

technical field [0001] The invention belongs to the field of environmental analytical chemistry, and relates to a method for synchronous derivatization of hydroxyketone groups of steroid environmental endocrine disruptors (estrone, 17β-estradiol, estriol, 17α-ethinyl estradiol and progesterone) , is the sample pretreatment method and core technology used by gas chromatography-mass spectrometry to analyze such substances. Background technique [0002] Environmental endocrine disrupting chemicals (Endocrine Disrupting Chemicals, EDCs), also known as environmental hormones (Environmental Hormones), refer to natural or artificial emissions in the environment, which can interfere or inhibit the endocrine system by simulating the physiological and biochemical effects in animals or humans. , and a large class of exogenous compounds that affect reproductive, nervous, and immune system functions. EDCs are highly toxic and bioaccumulative, and can interfere with the endocrine system ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J75/00C07J51/00G01N30/02G01N30/06G01N30/72
Inventor 潘学军方锴黄斌刘晶靓王宇高建培
Owner KUNMING UNIV OF SCI & TECH
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