Method for determining content of chloroalkane in chloral hydrate or preparation thereof

A technology for chlorinated alkanes and chloral hydrate, which is applied to measuring devices, instruments, scientific instruments, etc., can solve the problems of low detection sensitivity, poor reproducibility, and poor specificity of headspace gas chromatography, and achieve high accuracy and convenience. Operation, special effect

Active Publication Date: 2020-12-01
TEFENG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Headspace gas chromatography has low detection sen

Method used

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  • Method for determining content of chloroalkane in chloral hydrate or preparation thereof
  • Method for determining content of chloroalkane in chloral hydrate or preparation thereof
  • Method for determining content of chloroalkane in chloral hydrate or preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1 Chloroform, carbon tetrachloride and dichloromethane detection method

[0052] 1.1 Instruments and reagents

[0053] Instruments: gas chromatograph, GC-2014, Shimadzu Corporation, Japan; electronic analytical balance, CPA225D, Sartorius Scientific Instrument Co., Ltd., etc.

[0054] Reagent: reference substance chloroform, content is 98.1%, purchased from SIGMA-ALDRICH company, reference substance carbon tetrachloride content is 99.5%, concentration is 1002 μ g / ml (in methanol), purchased from BePure company; Chloromethane, with a content of 99.9%, was purchased from Dr. Ehrenstorfer GmbH; n-hexane was of mass spectrometry grade, the rest of anhydrous sodium sulfate and sodium chloride were of analytical grade, and water was self-made ultrapure water.

[0055] 1.2 Chromatographic conditions

[0056] Chromatographic column: capillary column (30m×0.53mm×3μm) with 6% cyanopropylphenyl-94% methylpolysiloxane as the stationary liquid;

[0057] Heating program...

Embodiment 2 3

[0074] Example 2 Chloroform detection method validation

[0075] overview

[0076] The detection method of chloroform was verified, and the verification results are summarized in Table 2.

[0077] Table 2 Summary of Trichloromethane Detection Method Validation

[0078]

[0079]

[0080] specific description

[0081] 2.1 Instruments and reagents

[0082] 2.1.1 Instruments

[0083] Table 3 Instruments and equipment

[0084] serial number equipment name model manufacturer 1 Gas Chromatograph GC-2014 Shimadzu Corporation 2 Gas Chromatograph 7890B Agilent Corporation 3 Electronic balance CPA225D Sartorius Scientific Instruments Ltd. 4 Electronic balance BSA224S Sartorius Scientific Instruments Ltd. 5 Electric constant temperature water bath DZKW-S-4 Beijing Guangming Medical Instrument Co., Ltd.

[0085] 2.1.2 Reagents

[0086] Chloral hydrate concentrate (74.48%, w / w), obtained from Xinjiang Tefeng Ph...

Embodiment 3 4

[0172] Embodiment 3 carbon tetrachloride detection method verification

[0173] overview

[0174] The detection method of carbon tetrachloride was verified, and the verification results are summarized in Table 12.

[0175] Table 12 Summary of carbon tetrachloride detection method verification

[0176]

[0177]

[0178] specific description

[0179] 3.1 Instruments and reagents

[0180] 3.1.1 Instruments and equipment

[0181] Table 13 Instruments and equipment

[0182] serial number equipment name model manufacturer 1 Gas Chromatograph GC-2014 Shimadzu Corporation 2 Electronic balance CPA225D Sartorius Scientific Instruments Ltd. 3 Electronic balance BSA224S Sartorius Scientific Instruments Ltd.

[0183] 3.1.2 Reagents

[0184] Chloral hydrate concentrate was obtained from Nanjing Tefeng Pharmaceutical Co., Ltd.;

[0185] The reference substance carbon tetrachloride, the content is 99.5%, the concentration is 1002 ...

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Abstract

The invention provides a method for determining the content of chloroalkane in chloral hydrate or a preparation thereof by gas chromatography, which comprises the following steps of 1, precisely weighing a chloroalkane reference substance, and dissolving the chloroalkane reference substance in an organic solvent to obtain a reference substance solution, 2, dissolving or diluting a to-be-detected sample chloral hydrate or a preparation thereof with water or an inorganic salt aqueous solution optionally, adding an organic solvent for extraction, and taking an organic layer as a test solution, and 3, respectively detecting the reference substance solution and the test solution through gas chromatography, and calculating the content of the chloralkane.

Description

technical field [0001] The application relates to a detection method for impurity content in medicines, in particular to a method for determining the content of chlorinated alkanes in chloral hydrate or its preparations by gas chromatography. Background technique [0002] Chloroform (CAS number: 67-66-3) has liver and kidney toxicity and potential carcinogenicity, and its content in medicines needs to be controlled. The 2015 edition of "Chinese Pharmacopoeia" and ICH Q3C stipulate that the limit of chloroform in raw materials is 60ppm. [0003] Carbon tetrachloride (CAS No.: 56-23-5) and dichloromethane (CAS No.: 75-09-2) belong to the first and second class of residual solvents respectively, and their amounts in pharmaceuticals also need to be controlled . [0004] The commonly used method for the determination of chlorinated alkanes is headspace gas chromatography. Headspace gas chromatography has low detection sensitivity, poor specificity, and poor reproducibility. ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N30/30G01N30/70
Inventor 云琦袁子惠吴小青
Owner TEFENG PHARM CO LTD
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