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LC-MS/MS法研究头孢美唑钠中有关物质
引用本文:孔兴欣,沈文斌,王丽云,石金芳,狄斌,张韬. LC-MS/MS法研究头孢美唑钠中有关物质[J]. 中国药科大学学报, 2012, 43(2): 170-176
作者姓名:孔兴欣  沈文斌  王丽云  石金芳  狄斌  张韬
作者单位:中国药科大学药物分析学教研室;中国药科大学分析测试中心;浙江亚太药业股份有限公司;中国药科大学药物分析学教研室;中国药科大学药物分析学教研室;浙江亚太药业股份有限公司
摘    要:
建立采用LC-MS/MS法对头孢美唑钠中有关物质进行定性分析。采用ODS色谱柱(250 mm×4.6 mm,5 μm),以1%甲酸水溶液-乙腈为流动相线性梯度洗脱;柱后分流,80%流出液经PDA检测,20%流出液电喷雾离子化MS测定。采集有关物质的PDA谱、质谱母离子及子离子谱,进行解析推测有关物质的结构。在所建立的条件下,头孢美唑钠及其有关物质分离良好,检测出8个有关物质,对其结构进行解析。建立的LC-MS/MS法有效地分离分析了头孢美唑钠及其有关物质,为其质量控制和工艺优化提供了技术参考。

关 键 词:头孢美唑钠;有关物质;LC-MS/MS;分析;鉴定

Identification of the related substances in cefmetazole sodium by LC-MS/MS
KONG Xing-xin,SHEN Wen-bin,WANG Li-yun,SHI Jin-fang,DI Bin and ZHANG Tao. Identification of the related substances in cefmetazole sodium by LC-MS/MS[J]. Journal of China Pharmaceutical University, 2012, 43(2): 170-176
Authors:KONG Xing-xin  SHEN Wen-bin  WANG Li-yun  SHI Jin-fang  DI Bin  ZHANG Tao
Affiliation:1Department of Pharmaceutical Analysis,Nanjing 210009;2Center for Instrumental Analysis,China Pharmaceutical University,Nanjing 210009;3Zhejiang Yatai Pharmaceutical Company,Shaoxing 312030,China
Abstract:
An LC-MS/MS method was established for the identification of the related substances in cefmetazole sodium.HPLC separation was carried out on an ODS column(250 mm×4.6 mm,5 μm)with a gradient elution with a mobile phase consisting of 1% formic acid aqueous solution and pure acetonitrile.80 percent of the eluent was monitored with PDA,and the rest was detected by tandem mass spectrometry.The PDA,parent ions and the corresponding product ions spectra of all the related substances in cefmetazole sodium were determined and elucidated.Good resolution of cefmetazole sodium and its main related substances was achieved.Eight related substances in cefmetazole sodium were detected by LC-MS/MS.The established method is effective in the separation and identification of the related substances in cefmetazole sodium and the results are useful for its quality control.
Keywords:cefmetazole sodium  related substances  LC-MS/MS  analysis  determination
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