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Method for determining dihydrotestosterone in medicine through derivatization HPLC method

A dihydrotestosterone and derivatization technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high cost of detection by mass spectrometry, many influencing factors of sample processing, and inability to detect drug components, etc., and achieve good sensitivity and accuracy High performance and simple method

Active Publication Date: 2019-04-16
GUANGDONG FOOD & DRUG VOCATIONAL COLLEGE
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  • Abstract
  • Description
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Problems solved by technology

[0008] To sum up, the reported methods for the determination of dihydrotestosterone, radioactive / enzyme-linked immunoassay are mainly used in clinical detection, and mass spectrometry is expensive, and there are two main problems: ①The operation process is cumbersome, and there are many factors affecting sample processing ; ② The determination sample is a biological sample, and the drug ingredients in the preparation cannot be detected

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  • Method for determining dihydrotestosterone in medicine through derivatization HPLC method
  • Method for determining dihydrotestosterone in medicine through derivatization HPLC method
  • Method for determining dihydrotestosterone in medicine through derivatization HPLC method

Examples

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Embodiment 1

[0068] Embodiment 1: Benzoyl chloride derivatization HPLC method measures the content of dihydrotestosterone in dihydrotestosterone medicine

[0069] In this embodiment, pyridine-benzoyl chloride is used as a derivatization reagent to benzoylate the hydroxyl group in the dihydrotestosterone molecule, and the RP-HPLC method is used for determination. Specific steps are as follows:

[0070] (1) Preparation of reference substance solution

[0071] Accurately weigh 10 mg of dihydrotestosterone reference substance, add 25 mL of methanol to dissolve it as the reference substance solution.

[0072] (2) Preparation of the test solution

[0073] Precisely weigh 1g of dihydrotestosterone gel (or 1g of dihydrotestosterone ointment or dihydrotestosterone cream or 1 bottle of dihydrotestosterone injection), extract with 30mL ethyl acetate for 10h under reflux, evaporate the ethyl acetate, and then use ethanol Reflux for extraction for 12 hours, recover ethanol, transfer the residue to a...

Embodiment 2

[0082] Embodiment 2: The content of dihydrotestosterone in dihydrotestosterone medicine is determined by p-nitrobenzoyl chloride derivatization HPLC method

[0083] In this example, dichloromethane-pyridine-p-nitrobenzoyl chloride was used as a derivatization reagent to benzoylate the hydroxyl group in the dihydrotestosterone molecule, and then determined by RP-HPLC. Specific steps are as follows:

[0084] (1) Preparation of reference substance solution

[0085] Accurately weigh 10 mg of dihydrotestosterone reference substance, add 25 mL of acetonitrile to dissolve as reference substance solution.

[0086] (2) Preparation of the test solution

[0087] Accurately weigh 1 g of dihydrotestosterone gel (or 1 g of dihydrotestosterone ointment or 1 g of dihydrotestosterone cream or 1 bottle of dihydrotestosterone injection), extract with 30 mL of ethyl acetate under reflux for 8 h, evaporate the ethyl acetate, take the filter residue and place In a conical flask, add 20 mL of met...

Embodiment 3

[0123] Embodiment 3: 3,5-dinitrobenzoyl chloride derivatization HPLC method measures the content of dihydrotestosterone in dihydrotestosterone medicine

[0124] In this example, pyridine-3,5-dinitrobenzoyl chloride was used as a derivatization reagent to benzoylate the hydroxyl group in the dihydrotestosterone molecule, and the RP-HPLC method was used for determination. Specific steps are as follows:

[0125] (1) Preparation of reference substance solution

[0126] Accurately weigh 10 mg of dihydrotestosterone reference substance, add 25 mL of acetonitrile to dissolve as reference substance solution.

[0127] (2) Preparation of the test solution

[0128] Precisely weigh 1 g of dihydrotestosterone gel or dihydrotestosterone ointment or dihydrotestosterone cream or 1 bottle of dihydrotestosterone injection, first reflux extraction with 30 mL of ethanol for 2 hours, filter, recover ethanol, take the filter residue and extract it three times with cyclohexane, 15 mL each time, c...

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Abstract

The invention relates to a method for determining dihydrotestosterone in a medicine through a derivatization HPLC method. The method comprises the steps that (1) a benzoyl halide compound is used as aderivatization reagent to carry out derivatization reaction on dihydrotestosterone in a medicine to be tested to acquire a sample containing a dihydrotestosterone derivatization product; and (2) a test solution is prepared by using the sample containing the dihydrotestosterone derivatization product, and the test solution is detected by high performance liquid chromatography, wherein the detectorof the high performance liquid chromatography is an ultraviolet detector. According to the invention, the method for determining dihydrotestosterone through derivatization HPLC-UVD is simple and versatile, and can be used for the determination of the medicine content in dihydrotestosterone preparations; and a methodology validation result shows that the method has the advantages of specificity, good sensitivity and high accuracy.

Description

technical field [0001] The invention relates to the field of drug analysis and detection, in particular to a method for determining dihydrotestosterone in drugs by a derivatization HPLC method. Background technique [0002] The types and contents of active ingredients contained in medicines are an important indicator of the quality of medicines, and the identification and testing of active ingredients is an effective means of drug quality control. A method commonly used in the separation and analysis of active ingredients of pharmaceuticals is High Performance Liquid Chromatography (HPLC). The main disadvantage of HPLC is the lack of detectors with high sensitivity and good versatility. Although ultraviolet detectors (Ultraviolet Detector, UVD) and fluorescence detectors (Fluorescence Detector, FLD) are widely used in HPLC, there are still some samples that cannot be detected. Because they have no UV chromophores or fluorophores. [0003] Micropenis is not uncommon in pedi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74G01N2030/067
Inventor 聂阳杨燕军朱俊访李博郭珅珅沈小莉丁立
Owner GUANGDONG FOOD & DRUG VOCATIONAL COLLEGE
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