Headspace gas chromatography method for determining residual quantity of organic solvent in glycine bulk drug

A headspace gas chromatography and organic solvent technology, applied in the field of headspace gas chromatography, can solve the problem of not measuring the residual amount of organic solvents in glycine raw materials

Inactive Publication Date: 2018-10-02
广西壮族自治区食品药品检验所
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the synthesis of glycine API, 12 organic compounds such as methanol, ethanol, acetone, isopropanol, acetonitrile, dichloromethane, ethyl acetate, n-propanol, tetrah...

Method used

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  • Headspace gas chromatography method for determining residual quantity of organic solvent in glycine bulk drug
  • Headspace gas chromatography method for determining residual quantity of organic solvent in glycine bulk drug
  • Headspace gas chromatography method for determining residual quantity of organic solvent in glycine bulk drug

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Experimental program
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Embodiment Construction

[0014] 1. Instruments and materials

[0015] 1.1 Instrument

[0016] Shimadzu GC-2010 gas chromatograph, including hydrogen flame ionization detector and HSS 8650 headspace sampler (Shimadzu, Japan), XS205 electronic balance (Switzerland METTLER TOLEDO).

[0017] 1.2 Materials

[0018] Glycine raw material (a company in Nanning, batch number: 8978170204, 8889750801, 8971170209), methanol, ethanol, acetone, isopropanol, acetonitrile, ethyl acetate, tetrahydrofuran, toluene (all purchased from Germany Merck company, the content is 99.9%, The batch numbers are 10894707725, AS1131-001, SA2SF11417, 151040, 1645868228, 160447, 1567531), n-propanol, dichloromethane, cyclohexane, n-butanol (all purchased from Sinopharm Chemical Reagent Co., Ltd., with a content of 99.5 %, the batch numbers are respectively 20170506, 20161110, 20160718, 20140213), and the water is ultrapure water.

[0019] 2. Methods and results

[0020] 2.1 Chromatographic conditions

[0021] Chromatographic colu...

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Abstract

The invention discloses a headspace gas chromatography method for determining the residual quantity of an organic solvent in a glycine bulk drug. The method is implemented under conditions that a DB-624 capillary column and a hydrogen flame ionization detector are used, sample inlet temperature is 150 DEG C, the detector temperature is 250 DEG C, high purity nitrogen is taken as carrier gas with flow rate being 2.2 mL/min, the split ratio is 10:1, headspace heating temperature is 80 DEG C, and equilibrium time is 35 min; besides, glycine is easily soluble in water and the 12 solvents are soluble in water to a certain degree, so that an aqueous solvent is adopted. The method can be used for simultaneously determining the residual quantity of the 12 organic solvents including methanol, ethanol, acetone, isopropanol, acetonitrile, dichloromethane, n-propanol, ethyl acetate, tetrahydrofuran, cyclohexane, n-butanol and toluene in the glycine bulk drug, has the characteristics of being easyto operate, quick, sensitive and accurate in result, and provides reference for effectively controlling the quality of the glycine raw material and ensuring medication safety.

Description

technical field [0001] The invention belongs to the technical field of quality detection of glycine raw materials, and in particular relates to a headspace gas chromatography method for determining residual organic solvents in glycine raw materials. Background technique [0002] Glycine, also known as aminoacetic acid, is an amino acid with the simplest structure and special sweetness. As an important fine chemical raw material, it is widely used in food, medicine, feed and other fields. Glycine is the basic raw material for the production of amino acids, and can be used as amino acid preparations, anti-gastric acid granules, and other excipients in the pharmaceutical industry. There are three main industrial production methods for glycine: natural protein hydrolysis, chloroacetic acid ammonium solution and St recker method. At present, the chloroacetic acid ammonium solution method is generally used in China, while the Strecker method is mainly used abroad. In the synthesi...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 李丹凤何虹黄慧罗意珊卢日刚朱健萍刘庄蔚朱荣
Owner 广西壮族自治区食品药品检验所
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