黄柏片中金胺O及重金属检查  

Study on the Method of Detecting Auramine-O,Tartrazineand Heavy Metal in Huangbai Tablets

作　　者：邓茂芝 周云峰 吴喆 邓杰华 黄炳泉 DENG Maozhi;ZHOU Yunfeng;WU Zhe;DENG Jiehua;HUANG Bingquan(Yichun Inspection and Testing Center,Yichun Jiangxi 336000,China)

机构地区：[1]宜春市检验检测中心,江西宜春336000

出　　处：《药品评价》2023年第11期1324-1327,共4页Drug Evaluation

基　　金：江西省药品监督管理局科研项目(2020JS25)。

摘　　要：目的建立黄柏片中金胺O的检查方法,同时考察该制剂中重金属残留水平。方法金胺O采用超高液相色谱串联质谱法(UPLC-MS/MS)进行分析,色谱柱为Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm),以乙腈-6 mmol/L乙酸铵溶液为流动相进行梯度洗脱,质谱离子源为电喷雾离子源(ESI),数据采集模式为多反应离子监测(MRM);重金属以汞、铅、铜、镉、砷、铬6种元素为分析指标,运用电感耦合等离子体质谱法(ICP-MS)对其含量进行测定。结果所有样品未检出金胺O;铅、汞、镉、砷、铜5种元素的含量低于标准要求,但有1批样品铬含量超过儿童服用拟定限量值。结论所建立的UPLC-MS/MS法可有效甄别黄柏片中是否存在金胺O,对重金属残留量的考察有助于评估其安全性。Objective To establish a method for the detection of auramine-O in huangbai tablets,and to investigate the residual level of heavy metal in the preparation.Methods The auramine-O was analyzed by UPLC-MS/MS on Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm)column with gradient elution using acetonitrile-0.1%formic acid solution as mobile phase.The mass spectrometry ion source was electrospray ion source(ESI),and the data acquisition mode was multi-reactive ion monitoring(MRM).Six elements including mercury,lead,copper,cadmium,arsenic and chromium were used as analysis indexes.Bismuth was used as internal standard for lead and mercury,chromium was used as internal standard for copper and arsenic,and indium was used as internal standard for cadmium.Their contents were determined by inductively coupled plasma mass spectrometry(ICP-MS).Results Auramine-O was not detected in all samples.The contents of 5 elements including lead,mercury,cadmium,arsenic and copper were lower than the standard requirements,but the content of chromium in one batch of samples exceeded the proposed limit for children.Conclusion The established UPLC-MS/MS method can effectively detect the presence of auramine-O in huangbai tablets,and the investigation of heavy metal residues is helpful to evaluate its safety.

关 键 词：黄柏 金胺O 重金属 超高液相色谱串联质谱法 电感耦合等离子体质谱法 

分 类 号：R286.0[医药卫生—中药学]