| 引用本文: | 冀峰,徐海英,李玮,陈振贺,董静,杨勇,李昕琦,阚家义,李晓东,曹磊.LCMS-QTOF鉴定卡络磺钠原料药的有关物质[J].中国现代应用药学,2022,39(7):934-941. |
| JI Feng,XU Haiying,LI Wei,CHEN Zhenhe,DONG Jing,YANG Yong,LI Xinqi,KAN Jiayi,LI Xiaodong,CAO Lei.Identification of Related Substances in Carbazochrome Sodium Sulfonate Raw Materials by LCMS-QTOF[J].Chin J Mod Appl Pharm(中国现代应用药学),2022,39(7):934-941. |
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| LCMS-QTOF鉴定卡络磺钠原料药的有关物质 |
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冀峰1, 徐海英2, 李玮3, 陈振贺1, 董静1, 杨勇2, 李昕琦4, 阚家义3, 李晓东1, 曹磊1
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1.岛津企业管理(中国)有限公司, 北京 100020;2.四川联成迅康医药股份有限公司, 成都 610091;3.安徽省食品药品检验研究院, 合肥 230051;4.成都天台山制药有限公司, 成都 611531
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| 摘要: |
| 目的 检测卡络磺钠原料药中有关物质，并进行结构鉴定，为工艺优化和质量控制提供参考。方法 采用Shim-pack Scepter C18(4.6 mm×250 mm，5 µm)色谱柱，以50 mmol·L–1乙酸铵水溶液为流动相A、乙腈为流动相B对卡络磺钠强制降解溶液中的有关物质进行分离。采用四极杆飞行时间高分辨质谱在m/z 100~800内进行正负离子扫描，数据依赖性采集获取二级质谱图。结合有关物质精确质量数、质谱裂解规律及卡络磺钠合成工艺推测其可能的结构。结果 卡络磺钠原料药经强制降解破坏得到8个主要的杂质，2种为已报道杂质，6种为本研究首次报道。强制降解试验表明卡络磺钠对高温和氧化相对较为稳定，光照、强酸和强碱条件对卡络磺钠影响较大。卡络磺钠原料药中检出杂质5，6和8，高温破坏的主要降解产物是杂质8。结论 本研究建立的液相色谱-四极杆飞行时间质谱联用法具有良好的分离能力，可有效地鉴定卡络磺钠原料药中有关物质，为其生产工艺和质量控制提供了参考。 |
| 关键词: 卡络磺钠 有关物质 四极杆飞行时间质谱 杂质谱 |
| DOI：10.13748/j.cnki.issn1007-7693.2022.07.012 |
| 分类号:R917.101 |
| 基金项目: |
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| Identification of Related Substances in Carbazochrome Sodium Sulfonate Raw Materials by LCMS-QTOF |
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JI Feng1, XU Haiying2, LI Wei3, CHEN Zhenhe1, DONG Jing1, YANG Yong2, LI Xinqi4, KAN Jiayi3, LI Xiaodong1, CAO Lei1
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1.Shimadzu(China) Co., Ltd., Beijing 100020, China;2.Sichuan Liancheng Xunkang Pharmaceutical Co., Ltd., Chengdu 610091, China;3.Anhui Institute for Food and Drug Control, Hefei 230051, China;4.Chengdu Tiantaishan Pharmaceutical Co., Ltd., Chengdu 611531, China
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| Abstract: |
| OBJECTIVE To detected the related substances in carbazochrome sodium sulfonate and indentified structure to provide reference for process optimization and quality control. METHODS The separation of related substances in forced degradation solution of carbazochrome sodium sulfonate was carried out by using a Shim-pack Scepter C18(4.6 mm×250 mm, 5 µm) with 50 mmol·L-1 ammonium acetate solution as mobile phase A and acetonitrile as mobile phase B. MS was performed on quadrupole time of flight high-resolution mass spectrometry under positive and negative mode with the mass range of m/z 100-800, MS2 was acquired under data dependent acquisition mode. Combined with the exact molecular mass, fragmentation rule and synthesis process, the possible structures of related substances were deduced. RESULTS Eight major impurities were found in carbazochrome sodium sulfonate degradation solutions. Among the identified impurities, 2 were reported and 6 were firstly reported. The force degradation test proved that carbazochrome sodium sulfonate was relatively stable on high temperature and oxidation conditions, while light, strong acids and strong alkali had a greater impact on carbazochrome sodium sulfonate. Related substances 5, 6 and 8 were detected in carbazochrome sodium sulfonate raw materials. Impurity 8 was the main degradation impurity by high temperature. CONCLUSION HPLC method combined with flight high resolution mass spectrometry established in this study has good separation and identification of related substances in carbazochrome sodium sulfonate, which provides a reference for its production process and quality control. |
| Key words: carbazochrome sodium sulfonate related substances LCMS-QTOF impurity profile |
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