超高效液相色谱-串联质谱法测定注射用头孢曲松钠中2-巯基苯并噻唑的含量  

Determination of 2-mercaptobenzothiazole in ceftriaxone sodium for injection by UPLC-MS/MS

作　　者：魏永涛 崔玉玲 林娣 张红梅 王桂英 张秋红 WEI Yongtao;CUI Yuling;LIN Di;ZHANG Hongmei;WANG Guiying;ZHANG Qiuhong(Jinan City Institute for Food and Drug Control,Jinan 250101,China;Shandong Freda Biotech Co.,Ltd.,Jinan 250101,China)

机构地区：[1]济南市食品药品检验检测中心,济南250101 [2]山东福瑞达生物股份有限公司,济南250101

出　　处：《分析试验室》2023年第11期1502-1507,共6页Chinese Journal of Analysis Laboratory

基　　金：山东省药品监督管理局质量风险专项([2022]174号)资助。

摘　　要：建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)测定注射用头孢曲松钠中2-巯基苯并噻唑(MBT)基因毒性杂质含量。样品经甲醇提取,50%(V/V)乙腈稀释后,采用ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,乙腈-0.05%(V/V)乙酸(80∶20,V/V)为流动相,电喷雾离子源(ESI),多反应监测(MRM)负离子模式扫描,外标法定量。MBT在0.11~10.92 ng/mL范围内线性关系良好(r^(2)=0.9989),检出限为0.03 ng/mL,定量限为0.08 ng/mL,平均回收率为96.8%,相对标准偏差(RSD)不大于3.5%。采用该方法检测抽检的14个厂家63批次样品中MBT杂质含量,59批次样品中有MBT检出。该方法适用于注射用头孢曲松钠中MBT的定性和定量分析。An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the determination of 2-mercaptobenzothiazole(MBT),a genotoxic impurity,in ceftriaxone sodium for injection.The extracts by methanol were dissolved and diluted with 50%(V/V)acetonitrile.The chromatographic separation was conducted on an ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8μm).The mobile phase was acetonitrile and water containing 0.05%(V/V)acetic acid with the proportion of 80∶20(V/V).The electrospray ionization(ESI)source in negative mode and multiple reaction monitoring(MRM)were used for the detection of MBT,and external standard method for quantitative analysis.The results showed that the proposed standard curve of MBT was linear in the range of 0.11-10.92 ng/mL,and the correlation coefficient(r^(2))was 0.9989.The limit of detection(LOD)was 0.03 ng/mL,and the limit of quantification(LOQ)was 0.08 ng/mL.The average recovery was 96.8%,and the relative standard deviation(RSD)was no higher than 3.5%.Samples of 63 batches from 14 pharmaceutical manufacturers were determined by this method,and MBTs were found in 59 batches.This method can be applied for the confirmation and detection of MBT in ceftriaxone sodium for injection.

关 键 词：注射用头孢曲松钠 2-巯基苯并噻唑 基因毒性杂质 超高效液相色谱-串联质谱法(UPLC-MS/MS) 

分 类 号：R917[医药卫生—药物分析学]