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Method for detecting residual solvent in medicine

A technology for residual solvents and drugs, applied in the field of detection of residual solvents in drugs, can solve problems such as qualitative determination of defects, and achieve the effects of simple assembly, easy promotion and saving test time.

Inactive Publication Date: 2008-06-25
NAT INST FOR THE CONTROL OF PHARMA & BIOLOGICAL PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still defects in the qualitative determination of each component in the detection sample and the determination of unknown impurity peaks and co-eluting peaks.

Method used

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  • Method for detecting residual solvent in medicine
  • Method for detecting residual solvent in medicine
  • Method for detecting residual solvent in medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 The establishment of residual solvent database

[0037] Instruments and software:

[0038] Trace GC Ultra (Thermo Electric Company); headspace system (Thermo Electric Company); figure 1 . Data analysis software is Xcalibur data processing system (Thermal Electric Company); Chromatographic column: SPB-1 type non-polar chromatographic column (30m × 0.32mm × 1um, Supelco company), HP-innowax type polar chromatographic column (30m × 0.32mm ×0.5um, Agilent)

[0039] Chromatographic conditions:

[0040]Temperature program: keep at 40°C for 8 minutes, then increase to 120°C at a rate of 8°C / min and hold for 10 minutes; inlet temperature: 200°C; constant flow rate: 4.0ml / min; carrier gas: helium; split ratio: 5 : 1; detector temperature: 250°C; headspace temperature: 70°C; headspace time: 20min.

[0041] Reagents: The reagents used were purchased from Aldrich Company, Fluka Company and Beijing Chemical Reagent Company, and the purity of all solvents was higher...

Embodiment 2

[0056] Determination of Residual Solvent in Example 2 Amoxicillin Sodium Clavulanate Potassium (5: 1)

[0057] The preparation of need testing solution: Accurately weigh 0.2384g of amoxicillin sodium clavulanate potassium (Korea Jingbao Pharmaceutical Co., Ltd., batch number D900400) (5:1), put in a 20ml headspace bottle, add 2.0ml water precisely, Seal the bottle tightly.

[0058] Preparation of butanone standard solution: Weigh 10 mg of butanone, put it in a 100ml volumetric flask, add water to the mark, measure 2ml, put it in a 20ml headspace bottle, and seal the mouth of the bottle.

[0059] Headspace condition and chromatographic condition are the same as embodiment 1, measure the retention time of butanone and the retention time of volatile components in need testing solution respectively, and calculate the chromatographic peak area, then compare with the database of embodiment 1 gained. See Table 3-1 and 3-2 for measurement results, Table 4-1 and 4-2 for content calcul...

Embodiment 3

[0075] Example 3 Determination of residual solvent in potassium clavulanate microcrystalline cellulose (1:1) The instruments and chromatographic conditions used are the same as those in Example 1.

[0076] Preparation of the test solution: accurately weigh 0.2139 g of potassium clavulanate microcrystalline cellulose (1:1), (Korea Jingbao Pharmaceutical Co., Ltd., batch number: D900400) put in a 20ml headspace bottle, and accurately add 2.0ml of water , Seal the mouth of the bottle.

[0077] Preparation of butanone standard solution: Weigh 10 mg of butanone, put it in a 100ml volumetric flask, add water to the mark, measure 2ml, put it in a 20ml headspace bottle, and seal the mouth of the bottle.

[0078] Headspace condition and chromatographic condition are the same as embodiment 2, measure the retention time of methyl ethyl ketone and the retention time of volatile component in need testing solution respectively, measure dead time with methane. The measurement results are sh...

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Abstract

The invention provides a qualitative and quantitative detection method of residual solvent in medicine through adopting a multi-channel parallel chromatographic column system in gas chromatography (GC), wherein, a double-channel or triple-channel shunt tube is arranged behind a gas chromatograph sampling system and in front of a chromatographic column; moreover, a chromatographic column of opposite polarity is connected in parallel behind the shunt tube, or a mass spectrum analysis system is connected with the shunt tube; in addition, each channel has an independent switch to control the switching on / off of the channel. According to the comparison and analysis of the detection result of the samples inside all channels, the method can complete the qualitative and quantitative analysis of the same sample at a time along with higher efficiency and accuracy.

Description

【Technical field】 [0001] The invention relates to the field of drug detection, in particular to a method for detecting residual solvents in drugs. 【Background technique】 [0002] Residual solvents in drugs refer to organic solvents used in the production of raw materials, excipients and preparations, but not completely removed during the process, such as benzene, carbon tetrachloride, acetonitrile, etc. When the level of residual solvent contained in the medicine is higher than the safe value, it will cause harm to the human body and the environment. [0003] On July 17, 1997, the International Council for Harmonization of Technical Requirements for Registration of Drugs for Human Use (ICH) passed the guidelines for the control of residual solvents in drugs, and classified 69 organic solvents commonly used in drug production according to the degree of harm to the human body and the environment. Four categories, and limits for each solvent are specified. At present, pharmac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/46G01N30/16
Inventor 胡昌勤刘颖尹利辉许明哲
Owner NAT INST FOR THE CONTROL OF PHARMA & BIOLOGICAL PROD
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