[1]赖树生 李 鑫 吴水华 陆 宇.LC-MS法测定托西酸舒他西林的聚合物杂质[J].大众科技,2021,23(6):24-26.
　Determination of the Polymer Impurities in Sultamicillin Tosylate by LC-MS[J].Popular Science & Technology,2021,23(6):24-26.
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LC-MS法测定托西酸舒他西林的聚合物杂质()
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《大众科技》[ISSN:1008-1151/CN:45-1235/N]

卷:
23
期数:
2021年6
页码:
24-26
栏目:
出版日期:
2021-06-20

文章信息/Info

Title:
Determination of the Polymer Impurities in Sultamicillin Tosylate by LC-MS
作者:
赖树生 李 鑫 吴水华 陆 宇
（广西中恒创新医药研究有限公司，广西 南宁 530031）
关键词:
液质联用; 杂质谱; 聚合物杂质; 托西酸舒他西林
Keywords:
liquid chromatograph-mass spectrometer (LC-MS) impurity spectrum polymer impurity sultamicillin tosylate
文献标志码:
A
摘要:
目的：开发适合液质联用的聚合物检测方法，考察托西酸舒他西林的聚合物杂质。方法：采用ZORBAX Eclipse Plus C18色谱柱（4.6 mm×100 mm，3.5 μm），以甲酸盐缓冲液（0.01 mol/L甲酸铵溶液，甲酸调节pH至3.0）为流动相A，乙腈为流动相B，梯度洗脱，流速1 mL/min；检测波长215 nm，柱温25℃，并联用质谱测试未知聚合物杂质峰的分子量。结果：在原料药杂质谱中识别出两个新聚合物杂质，分子量分别为721.2 m/z、926.3 m/z。结论：考察结果可为药品的质量控制提供参考。
Abstract:
Objective: To develop a LC-MS method for the determination of polymer impurities in sultamicillin tosilate. Methods: Zorbax eclipse plus C18 column (4.6 mm×100 mm, 3.5 μm) was used with formate buffer (0.01 mol/L ammonium formate, pH adjusted to 3.0 by formic acid) as mobile phase A and acetonitrile as mobile phase B. The flow rate was 1 mL/min with gradient elution. The detection wavelength was 215 nm and the column temperature was 25℃. The molecular weight of unknown polymer impurity was determined by mass spectrometry. Results: Two new polymer impurities were identified in the mass spectrum of active pharmaceutical ingredients with relative molecular mass of 721.2 m/z and 926.3 m/z. Conclusion: The results can provide reference for the quality control of drugs.

参考文献/References:

[1]　俞纯山. 舒他西林研究进展及其临床应用[J]. 广东医学，2000，21(1): 73-74. [2] 舒祝明，王建平. β-内酰胺类抗生素致敏原的产生及防范对策[J]. 医药导报，2004，23(5): 349. [3] 顾立素. 口服青霉素中致敏性高分子杂质的评价研究[D]. 北京: 中国协和医科大学，2005. [4] Kumar V J, Gupta P B, Kumar K S R P, et al. Identification, isolation and characterization of a new degradation product in sultamicillin drug substance[J]. Journal of Pharmaceutical and Biomedical Analysis, 2011, 54(3): 582-587. [5] 王勇跃. β-内酰胺类抗生素中高分子杂质检测新技术的应用研究[D]. 杭州: 浙江工业大学，2015. [6] 道客巴巴. European Pharmacopoeia 9.0[EB/OL]. http://www. doc88.com/p-07247376213506.html，2018-12-05.

备注/Memo

备注/Memo:
【收稿日期】2021-04-05 【作者简介】赖树生，广西中恒创新医药研究有限公司副总经理，工程师，研究方向为化药新药开发、化药质量控制。
更新日期/Last Update: 2021-09-14