基于HPLC-ICP-MS分析含雄黄外用制剂二黄栓中总砷及砷形态  

Analysis of total arsenic and elemental speciation of arsenic in an external preparation containing realgar Erhuang suppositories based on HPLC-ICP-MS

作　　者：苟欢 徐玲 姜涛 刘嵘[3] 方建国[1] 王文清 熊微 GOU Huan;XU Ling;JIANG Tao;LIU Rong;FANG Jianguo;WANG Wenqing;XIONG Wei(Department of Pharmacy,Tongji Hospital Affiliated with Tongji Medical College,Huazhong University of Science and Technology,Hubei Wuhan 430030,China;Hubei Institute for Drug Control/NMPA Key Laboratory for Quality Control of Chinese Medicine,Hubei Wuhan 430075,China;Department of Gynaecology,Tongji Hospital Affiliated with Tongji Medical College,Huazhong University of Science and Technology,Hubei Wuhan 430030,China)

机构地区：[1]华中科技大学同济医学院附属同济医院药学部,湖北武汉430030 [2]湖北省药品监督检验研究院/国家药品监督管理局中药质量控制重点实验室,湖北武汉430075 [3]华中科技大学同济医学院附属同济医院妇科,湖北武汉430030

出　　处：《中国医院药学杂志》2023年第23期2613-2617,共5页Chinese Journal of Hospital Pharmacy

基　　金：国家自然科学基金资助项目(编号:81403166);湖北省自然科学基金(编号:2019CFB744);国家药品监督管理局中药质量控制重点实验室(湖北)开放基金资助(编号:2022HBKFZ002)。

摘　　要：目的:建立二黄栓中总砷和砷形态的含量测定方法,探究其制备工艺和含量测定中影响砷形态转化的因素。方法:采用ICP-MS测定总砷及可溶性砷总量;高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定不同砷形态,结合多元统计分析影响砷形态转化的重要因素。结果:以硝酸为消解体系,梯度消解20 min能较好提取总砷;以2%磷酸溶液为提取溶剂,超声处理1 h能较好提取可溶性砷。总砷在1~200 ng·mL^(-1)范围内线性关系良好(r=0.9999),加样回收率为109.96%,RSD为0.95%(n=6);6种形态砷在5~200 ng·mL^(-1)范围内线性关系良好(r>0.9990),加样回收率为97.85%~113.64%,RSD<2.26%(n=6)。在多重线性回归分析模型中,制备工艺温度、含量测定提取方式和提取溶剂类型对砷形态转化具有显著影响。结论:该方法高效、准确,可用于二黄栓及含雄黄外用制剂中总砷含量及杂质限量的测定,揭示了影响砷形态转化的重要因素,对含雄黄制剂的研发制备及质量控制提供参考。OBJECTIVE To establish a method for the determination of total arsenic and arsenic speciation in Erghuang suppositories,and to explore the influencing factors in the transformation of arsenic speciation in the preparation process and content determination.METHODS ICP-MS was used to determine the contents of total arsenic and soluble arsenic.HPLC-ICP-MS was used to determine arsenic speciation.Combined with multivariate statistical analysis,the important factors affecting the transformation of arsenic speciation were analyzed.RESULTS Total arsenic could be completely extracted by gradient digestion with nitric acid for 20 min.With 2%phosphoric acid solution as the extraction solvent,the soluble arsenic could be extracted by ultrasonic treatment for 1 hour.The linearity was good within the range of total arsenic from 1 to 200 ng·mL~(-1)(r=0.9999),and the average recovery was 109.96%with the RSD of 0.95%(n=6);the linearity was good within the range of the six arsenic speciations from 5 to 200 ng·mL~(-1)(r>0.9990),and the average recovery ranged from 97.85%to 113.64%and the RSD was below 2.26%(n=6).In the multiple linear regression analysis model,preparation temperature,extraction method and solvent type had significant effects on arsenic speciation.CONCLUSION The method is efficient and accurate,and can be used for the quality control of arsenic in Erhuang suppositories and other external preparations containing realgar.It reveals the important factors in the transformation of arsenic speciation,and provides reference for the preparation and quality control of preparations containing realgar.

关 键 词：高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS) 二黄栓 雄黄 砷 形态 

分 类 号：R931.76[医药卫生—生药学]