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Method for separating and determining p-aminosalicylic acid and relevant impurities in LC-MSMS method

A technology of p-aminosalicylic acid and m-aminobenzenesulfonic acid, which is applied in the field of medicinal chemistry, can solve problems such as the inability of sensitivity to meet detection requirements, and achieves the effects of high sensitivity, good separation, and elimination of interference

Inactive Publication Date: 2018-07-27
CHONGQING HUABANGSHENGKAI PHARM
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  • Claims
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Problems solved by technology

The sensitivity of the conventional HPLC-UV method cannot meet the detection requirements. Therefore, it is urgent to provide a high-sensitivity method to detect genotoxicity warning structural impurities in aminosalicylic acid
[0011] At present, there is no method for the detection of m-aminobenzenesulfonic acid and m-nitrobenzenesulfonic acid by LC-MSMS. Therefore, providing a simple, high-resolution, and high-sensitivity method can more accurately ensure the detection of p-aminosalicylic acid and its preparations. Quality control, and finally determine the safety and effectiveness of the product

Method used

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  • Method for separating and determining p-aminosalicylic acid and relevant impurities in LC-MSMS method
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  • Method for separating and determining p-aminosalicylic acid and relevant impurities in LC-MSMS method

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Embodiment

[0065] LC-MSMS method for the separation and determination of p-aminosalicylic acid and its related impurities,

[0066] 1. Specific operation method:

[0067] Take 12.5mg of the test sample, weigh it accurately, put it in a 10ml measuring bottle, add 0.1ml N,N-dimethylacetamide, and accurately measure 1.0ml of the internal standard solution (take an appropriate amount of p-toluenesulfonic acid, accurately weigh , dissolve with 20% acetonitrile solution and quantitatively dilute to make a solution containing 10ng in every 1ml) put in a 10ml measuring bottle, dissolve with 20% acetonitrile solution and quantitatively dilute to the scale, shake up, as need testing solution; An appropriate amount of phenylbenzenesulfonic acid and m-aminobenzenesulfonic acid reference substance, accurately weighed, dissolved in 20% acetonitrile solution and quantitatively diluted to make a solution containing 10ng per 1ml, accurately measure 1.0ml of the solution, and put it in a 10ml measuring bo...

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Abstract

The invention belongs to the field of pharmaceutical chemistry, and particularly relates to a method for separating and determining p-aminosalicylic acid and relevant impurities in an LC-MSMS method.A chromatographic column adopted in the method adopts octylsilane bonded silicon gel as stuffing, adopts an acetic acid aqueous solution and an acetonitrile aqueous solution as mobile phases to perform the gradient elution, and performs the detection in a tandem mass spectrum detector; and the relevant impurities comprise m-nitrobenzenesulfonic acid and m-aminobenzenesulfonic acid. The method cansimultaneously detect the content of the m-nitrobenzenesulfonic acid and m-aminobenzenesulfonic acid in the p-aminosalicylic acid, and by screening the type of the mobile phase, optimizing the gradient of the mobile phase and selecting the chromatographic column, the interference on the p-aminosalicylic acid on the m-nitrobenzenesulfonic acid and m-aminobenzenesulfonic acid can be eliminated, so that the recovery rate with limit input is greater than 95 percent, and the detection limit reaches up to 0.4 ng / ml.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a method for separating and measuring p-aminosalicylic acid and related impurities by LC-MSMS. Background technique [0002] Tuberculosis is a chronic infectious disease caused by Mycobacterium tuberculosis infection. The Chinese name of Mycobacterium tuberculosis is Mycobacterium tuberculosis (M.tuberculosis). The cell wall of Mycobacterium tuberculosis contains lipids, which can prevent the loss of water in the bacteria, so it is particularly resistant to drying. Adhesions remain infectious for 8-10 days on dust and 6-8 months in dried sputum. Mycobacterium tuberculosis can undergo variations in morphology, colony, virulence, immunogenicity, and drug resistance. At present, rifampicin, isoniazid, ethambutol, and streptomycin are mostly used as the first-line drugs in the treatment of tuberculosis. Combination of rifampicin and isoniazid can reduce drug resistan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 颜波谭辉陈丽娜
Owner CHONGQING HUABANGSHENGKAI PHARM
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