A method for detecting impurities in tauroursodeoxycholic acid with high performance liquid chromatography

Abstract

The invention belongs to the technical field of drug quality determination methods, and in particular relates to a method for detecting impurities in tauroursodeoxycholic acid by high performance liquid chromatography. Impurity separation and limit requirements steps, in the test results, if ursodeoxycholic acid impurity ≤ 0.1%; taurochenodeoxycholic acid ≤ 0.1%, tauro nutria cholic acid ≤ 0.1%, p-nitrophenol ≤ 0.1% , the intermediate is less than or equal to 0.1%, it is a qualified quality product. The detection method in the present invention can comprehensively detect impurities in tauroursodeoxycholic acid under the same chromatographic conditions, so as to ensure the quality of the product; the operation is simple, the time is fast, the accuracy is high, the data is stable, and the cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of drug quality determination methods, in particular to a method for detecting impurities in tauroursodeoxycholic acid with a high performance liquid chromatography. Background technique [0002] Tauroursodeoxycholic acid (Tauroursodeoxycholic Acid) chemical name is 3α, 7β dihydroxycholanoyl-N-taurine, which is formed between the shuttle group of ursodeoxycholic acid (UDCA) and the amino group of taurine. The conjugated bile acid formed by shrinkage is white or off-white powder. Soluble in ethanol and methanol, soluble in glacial acetic acid, slightly soluble in water, insoluble in acetonitrile, ethyl acetate, acetone, tetrahydrofuran. It can increase the secretion of bile acids, lead to changes in the composition of bile acids, and increase their content in bile. Tauroursodeoxycholic acid can also inhibit the synthesis of cholesterol in the liver, reduce the amount of cholesterol and cholesterol esters in...

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Problems solved by technology

[0006] For example, in the description of Chinese patent CN201010552339.4, the impurity analysis method mentioned is a national standard chromatographic method, but this method cannot completely separate the relevant impurities.

In the description of Chinese patent 201010577534.2, a method for screening xanthine oxidase inhibitors by ultra-high performance liquid chromatography and mass spectrometry is also provided, but only a single impurity can be detected

There are also relevant literatures that mention "RP-HPLC method for the determination of related substances in ursodeoxycholic acid". This method also cannot separate all the impurities that need to be monitored; neither the domestic and foreign legal pharmacopoeias have recorded the impurity chromatogram of this product conditions; while the existing chromatographic conditions provided by the national standard can only monitor taurochenodeoxycholic acid impurities, other impurities that need to be monitored cannot be monitored under this chromatographic condition, but non-quantitative thin-layer chromatography (TLC ) for supplementation, such as taurine, ursodeoxycholic acid, other unknown impurities, etc.

However, due to the technical defects of these chromatographic conditions, it is impossible to meet the high-quality requirements of the product, and the multiple impurity monitoring methods increase the workload of quality monitoring personnel, and cannot monitor all impurities in the product in time, which is in line with the timely production monitoring requirements. performance, accuracy, etc. are very different

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