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Method for detecting multiple residual solvents in medicament

A drug and detector technology, which is applied in the detection field of gas chromatography, can solve the problem that the detection method cannot meet the demand, and achieves the effects of low accuracy requirements, simple operation and high accuracy

Active Publication Date: 2014-01-01
SHANGHAI NEW ASIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for simultaneously detecting multiple residual solvents in medicines, so as to overcome the defects that existing organic solvent detection methods cannot meet the demand

Method used

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  • Method for detecting multiple residual solvents in medicament
  • Method for detecting multiple residual solvents in medicament
  • Method for detecting multiple residual solvents in medicament

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] 1 Instruments and reagents

[0064] Agilent6890N gas chromatograph; Agilent7694E headspace sampler; cefotaxime sodium (batch number: TS0022); DMSO is HPLC grade, and other reagents are of analytical grade.

[0065] 2 Chromatographic conditions

[0066] Chromatographic column: capillary column with 100% polydimethylsiloxane as stationary liquid (HP-1 60m×530μm×5.00μm);

[0067] Carrier gas: N 2 ;

[0068] Ascending heating: keep at 40°C for 4 minutes, then start at 20°C˙min -1 The temperature is raised to 150°C at a rate of 6 minutes;

[0069] The inlet temperature is 200°C (split ratio: 1:1, column head pressure 7.70psi);

[0070] Detector: hydrogen flame ionization detector (FID);

[0071] Detector temperature: 250°C;

[0072] Headspace equilibrium temperature: 60°C;

[0073] Headspace equilibration time: 30min;

[0074] With DMSO as solvent.

[0075] 3 Preparation of solution

[0076] 3.1 Preparation of reference substance stock solution

[0077] Acc...

Embodiment 2

[0107] 1 Instruments and reagents

[0108] Agilent6890N gas chromatograph; Agilent7694E headspace sampler; meropenem sodium (batch number: FP005); DMSO was HPLC grade, and other reagents were of analytical grade.

[0109] 2 Chromatographic conditions

[0110] Chromatographic column: capillary column with 100% polydimethylsiloxane as stationary liquid (HP-1 60m×530μm×5.00μm);

[0111] Carrier gas: N 2 ;

[0112] Ascending heating: keep at 40°C for 8 minutes, raise the temperature to 150°C at a rate of 20°C / min, and hold for 8 minutes;

[0113] The inlet temperature is 200°C (split ratio: 1:1, column head pressure 7.70psi);

[0114] Detector: hydrogen flame ionization detector (FID);

[0115] Detector temperature: 250°C;

[0116] Headspace equilibrium temperature: 60°C;

[0117] Headspace equilibration time: 30min;

[0118] With DMSO as solvent.

[0119] Other steps are identical with embodiment 1.

[0120] 3 Solvent test results

[0121] Accurately measure ...

Embodiment 3

[0124] 1 Instruments and reagents

[0125] Agilent6890N gas chromatograph; Agilent7694E headspace sampler; cefoxitin (batch number: TX011); DMSO is HPLC grade, and other reagents are of analytical grade.

[0126] 2 Chromatographic conditions

[0127] Chromatographic column: capillary column with 100% polydimethylsiloxane as stationary liquid (HP-1 60m×530μm×5.00μm);

[0128] Carrier gas: N 2 ;

[0129] Ascending heating: keep at 40°C for 6 minutes, raise the temperature to 150°C at a rate of 20°C / min, and hold for 5 minutes;

[0130] The inlet temperature is 200°C (split ratio: 1:1, column head pressure 7.70psi);

[0131] Detector: hydrogen flame ionization detector (FID);

[0132] Detector temperature: 250°C;

[0133] Headspace equilibrium temperature: 60°C;

[0134] Headspace equilibration time: 30min;

[0135] With DMSO as solvent.

[0136] Other steps are identical with embodiment 1.

[0137] 3 Solvent test results

[0138] Precisely measure the cefoxiti...

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PUM

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Abstract

The invention relates to a method for detecting multiple residual solvents in a medicament. According to the method, by utilizing a gas chromatographic method, nine organic solvents including methanol, ethanol, acetonitrile, acetone, isopropanol, methylene dichloride, ethyl acetate, tetrahydrofuran and triethylamine in the medicament are simultaneously detected, the sensitivity and the precision are high, and the repeatability is good; by utilizing a standard addition method, other standard substances do not need to serve as internal standard substances, only pure substances of to-be-measured components are needed, the accuracy requirement on the sampling volume is low, and the operation is simple; by utilizing a headspace sampling method, a direct solution sample is prevented from interfering the detection and polluting a chromatographic column; by utilizing a temperature programming method, low-boiling-point organic solvents and high-boiling-point organic solvents can be effectively separated.

Description

technical field [0001] The invention relates to a detection method of gas chromatography, in particular to a method for simultaneously detecting multiple residual solvents in medicines. Background technique [0002] Drug residual solvents refer to volatile organic chemical substances used or generated during the production process of raw materials, excipients or preparations. These solvents that are not completely removed during the production process not only reduce the stability of the drug and affect the quality, but also increase the toxicity and carcinogenicity of the patient after taking it. The International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) classified 69 organic solvents commonly used in drug production and purification processes according to their degree of harm to the human body and the environment. into 4 categories. For the first, second and third types of solvents, the residual amount ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 郑玉林沈宏一姜文婷管海英
Owner SHANGHAI NEW ASIA PHARMA
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