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A High Performance Liquid Chromatographic Method for Derivative Detection of Steroidal Compounds A-ring Double Bond Isomers

A high-performance liquid chromatography and steroidal compound technology, applied in the field of drug analysis, can solve the problems of inability to achieve complete baseline separation, achieve good promotion and application prospects, good separation effect, and simple operation

Active Publication Date: 2019-05-21
CHENGDU XINJIE HIGH TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, experiments have shown that under the existing conventional liquid chromatography conditions, the two isomers cannot achieve complete baseline separation

Method used

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  • A High Performance Liquid Chromatographic Method for Derivative Detection of Steroidal Compounds A-ring Double Bond Isomers
  • A High Performance Liquid Chromatographic Method for Derivative Detection of Steroidal Compounds A-ring Double Bond Isomers
  • A High Performance Liquid Chromatographic Method for Derivative Detection of Steroidal Compounds A-ring Double Bond Isomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Instrument and chromatographic conditions:

[0060] Shimadzu LC-10AD high performance liquid chromatograph; the chromatographic column is a Techmate C18-ST chromatographic column (250mm×4.6mm×5μm); the column temperature is 30°C; the mobile phase is water-acetonitrile (55:45); The chromatographic liquid phase system is used for detection, the injection volume is 10 μL; the flow rate is 1.3ml / min; an ultraviolet detector is used; the detection wavelength is 200nm.

[0061] Experimental procedure

[0062] Derivation: Accurately weigh an appropriate amount of the sample and place it in a 25ml round bottom flask, accurately add an appropriate amount of dichloromethane to dissolve it, and then add m-chloroperoxybenzoic acid at a molar ratio of 1:1 to the sample. After reacting in a water bath at 25°C for 1 hour, remove the dichloromethane, and then accurately add an appropriate amount of acetonitrile to dissolve it, transfer it out, and obtain the product.

[0063] Prepara...

Embodiment 2

[0070] Instrument and chromatographic conditions:

[0071] Shimadzu LC-10AD high-performance liquid chromatography; the chromatographic column is Techmate C18-ST chromatographic column (250mm×4.6mm×5μm); the column temperature is 30°C; water-acetonitrile (55:45) is used as the mobile phase; Detection is performed with a high-performance chromatographic liquid phase system. The injection volume is 10 μL; the flow rate is 1.5 ml / min; an ultraviolet detector is used; the detection wavelength is 200 nm.

[0072] All the other operating steps and conditions are the same as in Example 1.

[0073] The test results show that the solvent peak has no interference to the isomers, and the peaks of the resolution solution isomers can be completely separated. See Figure 5 .

Embodiment 3

[0075] Instrument and chromatographic conditions:

[0076] Shimadzu LC-10AD high performance liquid chromatograph; the chromatographic column is a Techmate C18-ST chromatographic column (250mm×4.6mm×5μm); the column temperature is 35°C; the mobile phase is water-acetonitrile (55:45); Chromatographic liquid phase system for detection The injection volume is 10 μL; the flow rate is 1.3ml / min; an ultraviolet detector is used; the detection wavelength is 200nm.

[0077] All the other operating steps and conditions are the same as in Example 1.

[0078] The test results show that the solvent peak has no interference on the isomers, and the peaks of the resolution solution isomers can be completely separated, see Figure 6 .

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Abstract

The invention discloses a high performance liquid chromatography method used for derivative detection of steroid compound A ring double-bond isomers. The structures of the steroid compound A ring double-bond isomers are represented by formula I and II. The high performance liquid chromatography method comprises following steps: A, sample derivatization is carried out, wherein an isomer mixture is dissolved in an aprotic solvent, 3-chlorobenzoic acid or N-bromobutanimide is added, reaction is carried out at room temperature, and solvent volatilization is carried out; B, a mobile phase is used for dissolving a sample obtained via solvent volatilization, and 10<mu>l of an obtained solution is injected into a liquid chromatograph for detection; and C, high performance liquid chromatography is adopted to detect a sample solution obtained via derivatization, wherein octadecylsilane chemically bonded silica is taken as a filling material of an adopted chromatographic column, and mobile phase isocratic elution is adopted. The high performance liquid chromatography method can be used for separating and detecting steroid compound A ring double-bond isomers, and is high in detection precision and repeatability.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a high-performance liquid chromatography method for derivatizing and measuring the A-ring double-bond isomers of steroid compounds. Background technique [0002] 5α-Androst-2-en-17-one plays an important role in the field of medicine, especially in steroid hormones. Intermediates of ammonium bromide, pipecuronium bromide, rocuronium bromide, etc. [0003] 5α-androst-2-en-17-one, as an important intermediate of various drugs, will produce 3,4-double bond isomer, namely 5α-androst-3-en-17-one, during the synthesis process. Since the structure and polarity of 5α-androst-3-en-17-one and 5α-androst-2-en-17-one are very close, it is difficult to remove this impurity through purification or subsequent reaction. And because the reaction site and activity of 5α-androst-3-en-17-one and 5α-androst-2-en-17-one are similar to it, they will produce similar reactions with the same rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 李敏马欢欧世荣
Owner CHENGDU XINJIE HIGH TECH DEV CO LTD
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