| 引用本文: | 张拥军,梁紫琦,郭拥政,朱勇华,周文武,王书芳.LC-MS同时测定醋酸卡泊芬净中的3种杂质[J].中国现代应用药学,2023,40(24):3418-3422. |
| ZHANG Yongjun,LIANG Ziqi,GUO Yongzheng,ZHU Yonghua,ZHOU Wenwu,WANG Shufang.Simultaneous Determination of Three Impurities in Caspofungin Acetate by LC-MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2023,40(24):3418-3422. |
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| LC-MS同时测定醋酸卡泊芬净中的3种杂质 |
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张拥军1, 梁紫琦2, 郭拥政1, 朱勇华1, 周文武1, 王书芳2,3
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1.浙江野风药业股份有限公司, 浙江 东阳 322100;2.浙江大学金华研究院转化药学创制中心, 浙江 金华 321016;3.浙江大学药学院, 杭州 310058
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| 摘要: |
| 目的 建立同时测定醋酸卡泊芬净中杂质A、C和D的LC-MS方法。方法 色谱柱为Waters CORTECS® C18+（4.6 mm×150 mm，2.7 μm）色谱柱；流动相A为0.1%甲酸-水溶液，流动相B为0.1%甲酸-乙腈；用电喷雾离子化单四极杆质谱，以选择离子检测方式对杂质A和C进行正离子检测，对杂质D进行负离子检测。结果 杂质A、C和D在线性范围内线性系数r≥0.9993；平均回收率分别为100.5%，104.1%和105.2%，RSD<4%（n=6）；按S/N=10计算，杂质A、C和D的定量限分别为31.8，6.99，15.5 ng·mL–1。3批样品中杂质A、C和D的含量均低于限度值。结论 该方法简单、灵敏度高、适用性强，可用于醋酸卡泊芬净中杂质A、C和D的同时定量检测，并可为醋酸卡泊芬净中其他杂质检测提供参考。 |
| 关键词: 醋酸卡泊芬净 杂质 液相色谱-质谱联用 |
| DOI：10.13748/j.cnki.issn1007-7693.20231194 |
| 分类号:R917.101 |
| 基金项目: |
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| Simultaneous Determination of Three Impurities in Caspofungin Acetate by LC-MS |
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ZHANG Yongjun1, LIANG Ziqi2, GUO Yongzheng1, ZHU Yonghua1, ZHOU Wenwu1, WANG Shufang2,3
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1.Zhejiang Wild Wind Pharmaceutical Co., Ltd., Dongyang 322100, China;2.Innovation Center of Translational Pharmacy, Jinhua Institute of Zhejiang University, Jinhua 321016, China;3.College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China
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| Abstract: |
| OBJECTIVE To develop LC-MS method for the simultaneous determination of impurities A, C, and D of caspofungin acetate. METHODS Waters CORTECS® C18+(4.6 mm×150 mm, 2.7 μm) was used as the chromatography column. Mobile phase A and B were 0.1% formic acid-H2O and 0.1% formic acid-CH3CN, respectively. Electrospray ion source-single quadrupole mass spectrometry was used to detect impurities A and C in positive ion mode and impurity D in negative ion mode. RESULTS The correlation coefficient r was ≥ 0.9993 in linearity ranges of impurities A, C and D. The average recoveries were 100.5%, 104.1% and 105.2%, respectively, with RSD<4%(n=6). The LOQs (S/N=10) of impurities A, C and D were 31.8, 6.99 and 15.5 ng·mL-1 respectively. The contents of impurities A, C and D in the three samples were all below the limits. CONCLUSION The developed LC-MS method is simple, sensitive, and applicable, which can be used to simultaneously determine impurities A, C and D in caspofungin acetate and can also provide a reference for the detection of other impurities in caspofungin acetate. |
| Key words: caspofungin acetate impurity LC-MS |
