注射用苯磺顺阿曲库铵有关物质的LC-MS初步鉴定.pdfVIP

申晴..带九攀学报 Joumal of China Pharmaceutical University 2013 ,44( 1) :65 -72 65 注射用苯磺JI阪阿曲库按有关物质的 LC-MS 初步鉴定 张璐1 ， 2 ，强淑萍1 ，张云静1 ，王磊2 ，张晓飞2 ，杭大俊1 • e 中国药科大学药物分析学教研室，南京 210∞9;2东英(江苏)药业有限公司，南京 21∞19) 摘 要 采用高效液相色谱·高分辨质诱联用技术对注射用苯磺顺阿曲库练中有关物质进行初步结构鉴定。采用 SEPAX GP-C 1s (250 mmx4.6 mm ,5 J.Lm) 色谱柱，水·乙蜻·甲醇·甲酸(650: 175: 175: 10 ,1. 010 L 中含甲酸铃1. 3 g) 流动相等 度洗脱，对注射用苯磺顺阿曲库钱有关物质进行分离;采用 LC/TOF-MS 测定各有关物质的准确质量，电喷雾离子化 LC­ MS/MS 进行结构解析。共检测出 11 个有关物质，其中 7 个的含量在0.1% 以上，并初步鉴定了它们的结构，其中 5 个有关 物质在已有药典标准中未明确规定。 关键词 苯磺顺阿曲库馁;有关物质;结构鉴定;LC/TOF-MS;LC-MS/MS 中圄分类号 R917 文献标志码 A 文章编号 1∞0-5048(2013)01 -∞65 -08 Preliminary identification of the related substances in cisatracurium besylate for i 时ection by LC-MS I 2 l l 2 l ZHANG LU • , QIANG Shuping , ZHANG Yunjing , WANG Lei , ZHANG Xiaofee , HANG Taijun JDepartment 01 p加， rmaceutical Analys白， China p阳， mωceωical University, Nanji略2刷刷; 2 Dongying (Jiangsu) Pharmaceutical Co. ， μd. , Nanjing 21ω19， China Abstract Hyphenated methods of chromatography and high resolution mass spectrometηwere established for the identification of the related substances in cisatracurium besylate for injection. The analysis was conducted on SEPAX GP-C I8 column by isocratic elution using a mixture of water , acetonitrile , methanol , formic acid and ammonium formate in the ratio of 650 : 175 : 175 : 10 : 1. 3 as the mobile phase at the flow rate of 1. 0 ml/ min. The related substances were detected and identified by LC/TOF-MS and LC-MS/MS with acetonitrile aided electrospray ionization. Eleven related substances were found in cisatracurium besylate for injection , seven of which had the area normalization content of over O. 1%. Based on the structural character