Method for determining chloral hydrate content by high performance liquid chromatography

A chloral hydrate and high-performance liquid chromatography technology, which is applied in the field of chloral hydrate content, can solve the problems of inaccurate chloral hydrate, lack of specificity and accuracy, and achieve the goals of saving organic solvents, easy operation, and cost reduction Effect

Active Publication Date: 2019-08-23
TEFENG PHARM CO LTD
View PDF3 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because chloral hydrate in the preparation can be degraded to generate chloroform and chloral, so the amount of indirect determination of chloroform and chloral can not accurately reflect the amount of chloral hydrate in the product, direct sample gas chromatography and headspace gas chromatography Does not have good specificity and accuracy

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for determining chloral hydrate content by high performance liquid chromatography
  • Method for determining chloral hydrate content by high performance liquid chromatography
  • Method for determining chloral hydrate content by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0023] (1) Preparation of reference substance solution and need testing solution: accurately weigh an appropriate amount of chloral hydrate reference substance, dissolve it with mobile phase to make a reference substance solution of specified concentration; accurately weigh an appropriate amount of chloral hydrate test substance, and Dissolve or dilute and constant volume, obtain need testing solution; Wherein said mobile phase is acetonitrile-water;

[0024] (2) Determination: The reference substance solution and need testing solution are carried out liquid chromatography detection, record chromatogram, according to reference substance solution concentration, peak area and need testing solution peak area, external standard method calculates in the need testing solution Chloral hydrate content.

[0025] In some embodiments, the calculation formula is as follows:

[0026]

[0027] in

[0028] A 供试品 refers to the peak area of ​​the test solution;

[0029] A 对照品 refers to...

Embodiment 1

[0081] In the present embodiment, measure the content of chloral hydrate through the following steps:

[0082] (1) Preparation of reference substance solution and need testing solution: Accurately weigh 25.02 mg of chloral hydrate reference substance, put it in a 25ml measuring bottle, add mobile phase (acetonitrile: water=10:90) to dissolve and dilute to the scale, as Reference solution (C 对照品 =1.0128mg / ml); Precision takes by weighing chloral hydrate crude drug 23.63mg, puts in 25ml measuring bottle, adds mobile phase (acetonitrile: water=10: 90) to dissolve and be diluted to scale, obtain need testing solution (chlorine hydrate The aldehyde concentration is about 1 mg / ml);

[0083] (2) measure: described reference substance solution and need testing solution are measured according to following chromatographic conditions, record chromatogram (such as figure 1 Shown), according to reference substance solution concentration, peak area and need testing product peak area, calc...

Embodiment 2

[0096] Example 2: Methodological Validation

[0097] According to the "Chinese Pharmacopoeia" 2015 edition appendix (9101) drug quality standard analytical method validation guidelines and ICH analytical method validation guidelines for methodological validation, the process and results are as follows:

[0098] Solution preparation

[0099] Preparation of reference stock solution

[0100] Take about 0.1 g of the chloral hydrate reference substance, accurately weigh it, put it in a 50ml measuring bottle, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the reference substance stock solution.

[0101] Preparation of reference solution

[0102] Take about 25mg of chloral hydrate reference substance, weigh it accurately, put it in a 25ml measuring bottle, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the reference substance solution.

[0103] Preparation of the test solution

[0104] Get about 1g of chloral hydrate...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to view more

Abstract

The invention discloses a method for determining chloral hydrate content by high performance liquid chromatography. The method includes the following steps: (1) a step of preparation of a reference solution and a test solution, namely a step of precisely weighing an appropriate amount of a chloral hydrate reference substance, dissolving the reference solution prepared into a specified concentration by a mobile phase, precisely weighting an appropriate amount of chloral hydrate as a tested object, dissolving the chloral hydrate test solution by the mobile phase and carrying out volume fixing toobtain the test solution, wherein the mobile phase is acetonitrile-water; and (2) a step of determination, namely a step of carrying out liquid chromatography on the reference solution and the test solution, recording a chromatogram, and calculating the content of the chloral hydrate in the tested object by an external standard method according to a peak area and concentration of the reference substance and a peak area of the tested object. The method provided by the invention has good specificity and accuracy compared with a gas chromatography method and a titration method, saves organic solvents, reduces cost, is convenient in operation, meets the requirements of medical analysis methods in Chinese Pharmacopoeia, and has important application value in the quality research of raw medicine and preparations and other aspects.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for measuring the content of chloral hydrate in solid or liquid samples by high performance liquid chromatography. Background technique [0002] Chloral hydrate, chemical name 2,2,2-trichloro-1,1-ethylene glycol, English name Chloral hydrate, CAS No. 302-17-0, chemical structural formula: [0003] [0004] Chloral hydrate is easy to degrade under conditions such as heat, oxidation, and light, and its properties are unstable, especially poor stability in aqueous solution. Chloral hydrate slowly decomposes in aqueous solution, and decomposes faster during heating, oxidation and light, and generates degradation products such as chloroform, dichloroacetaldehyde, trichloroacetic acid, hydrochloric acid (Nanjing Municipal Health Bureau, hospital preparation specification [M]. Jiangsu : Nanjing University Press, 1989: 146). Various degradation products will affect th...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74G01N30/00
Inventor 云琦陶亮唐城李月荣
Owner TEFENG PHARM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap