登录    |    注册

您好,欢迎来到中国测试科技资讯平台!

首页> 《中国测试》期刊 >本期导读>ICP-MS测定5种中药注射液中重金属及有害元素

ICP-MS测定5种中药注射液中重金属及有害元素

161    2020-01-19

免费

全文售价

作者:张春华, 陈春桃, 韩必恺, 李子宜, 陈亮, 朱志鑫, 吴惠勤, 黄晓兰

作者单位:中国广州分析测试中心 广东省分析测试技术公共实验室 广东省中药质量安全工程技术研究中心, 广东 广州 510070


关键词:电感耦合等离子体质谱法;中药注射液;重金属及有害元素;直接稀释法


摘要:

建立电感耦合等离子体质谱法(ICP-MS)测定复方蒲公英注射液、野菊花注射液、肿节风注射液、白花蛇舌草注射液和夏天无注射液中铜(Cu)、砷(As)、镉(Cd)、铅(Pb)和汞(Hg)5种重金属及有害元素含量的方法。样品用2%硝酸(V/V)直接稀释,以72Ge、115In、185Re为内标,采用ICP-MS测定溶液中元素含量。方法学验证表明:Cu、As、Cd、Pb在0.5~50 μg/L和Hg在0.5~10 μg/L的质量浓度范围内线性关系良好(r2>0.999);低、中、高3种浓度水平,复方蒲公英注射液、夏天无注射液、肿节风注射液、野菊花注射液、白花蛇舌草注射液中5种元素的平均回收率(n=3)分别为90.7%~121.2%、83.4 %~119.9%、90.8%~116.3%、86.4%~109.0%、85.0%~118.0%,重复性RSD(n=3)分别为1.4%~9.8%、0.2%~6.7%、0.4%~7.4%、0.6%~10.0%、0.1%~11.1%;5种注射液中Cu、As、Cd、Pb、Hg的LOQ分别为0.002 1 mg/L、0.001 6 mg/L、0.000 56 mg/L、0.001 8 mg/L、0.001 7 mg/L,满足方法学验证的要求。各3批次实际中药注射液样品的测试结果表明,5种元素含量均小于限量值,说明其安全风险较小。方法操作简便、快速、灵敏度高、准确度好,适合5种注射液中的Cu、As、Cd、Pb、Hg等有害元素含量的测定,为其他中药注射液中元素杂质分析方法的建立提供参考。


Determination of heavy metals and harmful elements in five traditional Chinese medicine injections using inductively coupled plasma mass spectrometry (ICP-MS)
ZHANG Chunhua, CHEN Chuntao, HAN Bikai, LI Ziyi, CHEN Liang, ZHU Zhixin, WU Huiqin, HUANG Xiaolan
Guangdong Provincial Public Laboratory of Analysis and Testing Technology, Guangdong Engineering and Technology Research Center for Quality and Safety of Traditional Chinese Medicine, China National Analytical Center, Guangzhou, Guangzhou 510070, China
Abstract: A method for the determination of heavy metals and harmful elements(Cu, As, Cd, Pb, Hg) in five traditional Chinese medicine injections using inductively coupled plasma mass spectrometry (ICP-MS) was developed and validated. The traditional Chinese medicine injections was pretreated by diluting with 2% nitric acid (V/V), then the five target elements and internal standard elements (72Ge, 115In, 185Re) were detected by ICP-MS. The established method was fully validated. The calibration curves were linear over a range of 0.5-50 μg/L for Cu, As, Cd, Pb, and 0.5-10 μg/L for Hg, and the correlation coefficients (r2) were higher than 0.999. At three spiked levels (low, medium and high concentration), the average recoveries (n=3) for the five elements in Fufang Pugongying injection, Xiatianwu injection, Zhongjiefeng injection, Yejuhua injection, Baihuasheshecao injection were 90.7%-121.2%, 83.4%-119.9%, 90.8%-116.3%, 86.4%-109.0%, 85.0%-118.0%, respectively, with the RSDs (n=3) were 1.4%-9.8%, 0.2%-6.7%, 0.4%-7.4%, 0.6%-10.0%. 0.1%-11.1%. The limits of quantitation (LOQ) for Cu, As, Cd, Pb, Hg in five traditional Chinese medicine injections were 0.002 1, 0.001 6, 0.000 56, 0.001 8, 0.001 7 mg/L. Three batches of five actual traditional Chinese medicine injections were analyzed using the developed method, and the results showed that the contents of Cu, As, Cd, Pb and Hg were all less than the limits. The method, proved to be easy to handle, rapid and sensitive, meets the method validation requirements, and was suitable for the determination of the heavy metals and harmful elements in five traditional Chinese medicine injections. It also can supply a reference for the determination of the elemental impurities in the other traditional Chinese medicine injections
Keywords: inductively coupled plasma mass spectrometry (ICP-MS);traditional Chinese medicine injections;heavy metals and harmful elements;direct dilution
2020, 46(1):71-76  收稿日期: 2019-08-01;收到修改稿日期: 2019-09-26
基金项目: 2017年工业转型升级(中国制造2025)资金项目(工信部规[2017]333号)
作者简介: 张春华(1987-),男,福建三明市人,助理研究员,硕士,主要从事分析化学工作
参考文献
[1] 李瑞宏, 沈立茹, 张古英, 等. 某儿童医院132例中药注射剂不良反应报告分析[J]. 中国药业, 2019, 28(11):120-123
[2] ICH:ICH Q3D (R1) Guideline for Elemental Impurities[EB/OL]. (2019-03-22)[2019-06-03]. https://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q3D/Q3D-R1EWG_Document_Step4_Guideline_2019_0322.
[3] 扈福, 扈晓雯. 从中药注射剂说明书思考用药安全性问题[J]. 中国药房, 2009, 20(36):2879-2880
[4] 刘春平, 易智彪. 关于中药注射剂研究开发及安全性问题的思考[J]. 中草药, 2009, 40(7):1162-1166
[5] 林红梅, 周刚, 王停. 中药注射剂新药研发策略分析[J]. 中国新药杂志, 2019, 28(8):897-902
[6] 中国国家药典委员会, 中华人民共和国药典(2015年版四部)[M]. 北京:中国医药出版社, 2015.
[7] 聂黎行, 金红宇, 王钢力, 等. 4种中药注射液中重金属及有害元素残留量检测方法研究[J]. 中国中药杂志, 2008, 33(23):2764-2767
[8] 李耀磊, 张志成, 金红宇, 等. ICP-MS法测定复方苦参注射液中铜、砷、镉、汞、铅元素的残留量[J]. 药物分析杂志, 2018, 38(10):1781-1787
[9] 黄训瑞. ICP-MS法测定生脉注射液中5种重金属元素的含量[J]. 中国药房, 2014, 25(17):1619-1621
[10] 李丽敏, 王柯, 季申. 电感耦合等离子质谱法测定肾康注射液中重金属及有害元素[J]. 药物分析杂志, 2012, 32(02):277-281
[11] 施晓光, 赵庄, 陆敏仪, 等. 微波消解ICP-MS法测定黄芪注射液中5种重金属元素含量[J]. 中国药师, 2013, 16(04):494-496
[12] 张静娇, 姜范成, 郑尚季, 等. ICP-MS法测定6种中药注射液中重金属含量研究[J]. 中国药物评价, 2017, 34(3):165-167
[13] 严赟, 张赟赟. ICP-MS测定4种中药注射液中35种微量元素[J]. 中国新药杂志, 2016, 25(15):1778-1783
[14] 刘庄蔚, 王娟. 微波消解-ICP-MS法测定血栓通注射液中20种元素[J]. 中成药, 2016, 38(10):2188-2191
[15] 郭红丽, 张硕, 刘利亚, 等. ICP-MS法测定注射用灯盏花素等10种常用中药注射剂中13种金属元素[J]. 中草药, 2015, 46(17):2568-2572