Separation analysis method of residual amount of chloroform in meclizine dihydrochloride

A technology for the separation and analysis of meclizine hydrochloride, which is applied in the direction of material separation, analysis materials, and measuring devices, can solve the problems of low chloroform response value and inability to accurately measure chloroform residues, and achieve high sensitivity, easy operation, and responsiveness. high value effect

Active Publication Date: 2014-01-29
NEW FOUNDER HLDG DEV LLC +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chloroform has been detected by the flame ionization detector (FID) method in other pharmaceutical compounds, but the inventors have found that the response

Method used

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  • Separation analysis method of residual amount of chloroform in meclizine dihydrochloride
  • Separation analysis method of residual amount of chloroform in meclizine dihydrochloride
  • Separation analysis method of residual amount of chloroform in meclizine dihydrochloride

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experiment example 1

[0104] Experiment name: Optimization of chromatographic conditions for the determination of chloroform residues in meclizine hydrochloride

[0105] Purpose of the experiment: Determination of chloroform residues in meclizine hydrochloride, optimization of column temperature conditions

[0106] Experimental method: Agilent 7820A gas chromatograph, Agilent 7694E headspace sampler. A capillary column (30m×0.53mm×3.0μm) using (6%) cyanopropylbenzene-(94%) dimethyl polysiloxane copolymer as the stationary phase, an electron capture detector (ECD), and a detector The temperature is 300°C, the temperature of the injection port is 250°C, the carrier gas is nitrogen, and the flow rate of the carrier gas is 3ml per minute;

[0107] Chromatographic column temperature: use 100°C, 80°C, 60°C, 45°C respectively, and maintain for 6-15 minutes;

[0108] Last run at 200°C, maintain for 5 minutes; or do not set the last run program;

[0109] Headspace equilibration time 10, 15, 30, 60 minute...

experiment example 2

[0122] Experiment name: Method validation for chloroform residues in meclizine hydrochloride—linearity test

[0123] The purpose of the experiment: to verify the linear range of the method for the residual amount of chloroform in meclizine hydrochloride through a linear test

[0124] Experimental method: Agilent 7820A gas chromatograph, Agilent 7694E headspace sampler. A capillary column (30m×0.53mm×3.0μm) using (6%) cyanopropylbenzene-(94%) dimethyl polysiloxane copolymer as the stationary phase, an electron capture detector (ECD), and a detector Temperature 300°C, inlet temperature 250°C, carrier gas nitrogen, carrier gas flow rate 3ml per minute; column temperature: 45°C for 15 minutes, then run at 200°C for 5 minutes; headspace equilibration time 30 minutes.

[0125] Take about 16.5mg of chloroform, accurately weigh it, put it in a 25ml measuring bottle, dilute to the mark with methanol, shake well, and use it as a concentrated solution. Accurately measure appropriate am...

experiment example 3

[0131] Experiment Name: Method Validation for Chloroform Residues in Meclizine Hydrochloride—Lowest Limit of Detection and Limit of Quantification

[0132] Experimental purpose: To verify the sensitivity of the method for chloroform residues in meclizine hydrochloride through the lowest detection limit and the lowest quantification limit.

[0133] Experimental method: Agilent 7820A gas chromatograph, Agilent 7694E headspace sampler. A capillary column (30m×0.53mm×3.0μm) using (6%) cyanopropylbenzene-(94%) dimethyl polysiloxane copolymer as the stationary phase, an electron capture detector (ECD), and a detector Temperature 300°C, inlet temperature 250°C, carrier gas nitrogen, carrier gas flow rate 3ml per minute; column temperature: 45°C for 15 minutes, then run at 200°C for 5 minutes; headspace equilibration time 30 minutes.

[0134] Take the 0.66μg / ml solution in the chloroform linearity test, dilute it step by step with methanol, and determine the lowest detection limit an...

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Abstract

The invention discloses a separation analysis method of the residual amount of chloroform in meclizine dihydrochloride. The separation analysis method is characterized in that a gas chromatographic (GC) method and an electron capture detector (ECD) are used for the separation analysis of the residual amount of the chloroform in the meclizine dihydrochloride. The separation analysis method can be used for overcoming the shortcoming that when a gas chromatographic method of a conventional flame ionization detector (FID) is used for detection, the response value of the chloroform is low, has the advantages that the response value of the chloroform is high, the sensitivity is high, and the operation is simple and convenient, and provides technical reference for the establishment of the quality standard for the residual amount of chloroform in medicinal raw materials.

Description

technical field [0001] The invention relates to a method for separating and analyzing samples. In particular, it relates to a method for separation and analysis of residual chloroform in meclizine hydrochloride. Background technique [0002] The chemical name of meclizine hydrochloride is 1-[(4-chlorophenyl)benzyl]-4-[(3-methylphenyl)methyl]-piperazine dihydrochloride; the English name is 1-[ (4-Chlorophenyl)-phenylmethyl]-4-[(3-methylphenyl)methyl]piperazine dihydrochloride; molecular formula is C 25 h 27 ClN 2 2HCl; the molecular weight is 463.88; the chemical structural formula is shown in formula I below: [0003] [0004] Meclizine hydrochloride is a drug recorded in the Chinese Pharmacopoeia (2010 edition), CAS number: 1104-22-9, is an antagonist of histamine receptors, suitable for various skin and mucous membrane allergies, and can also be used for pregnancy, radiotherapy Nausea and vomiting caused by motion sickness. Its effect is far longer than that of di...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 易崇勤兰静郭欲晓郑少辉苏强
Owner NEW FOUNDER HLDG DEV LLC
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