摘要
目的:建立复方苦参注射液中铜、砷、镉、汞、铅5种元素残留量的测定方法。方法:样品经消解后采用电感耦合等离子体质谱法(ICP-MS法)测定,射频功率为1 550 W,载气(高纯氩气)流速为1.05L·min^(-1),等离子气体流速为15.0 L·min^(-1),蠕动泵转速0.2 r·s^(-1),采样深度10 mm,重复次数为3次。通过在线加入内标锗、铟、铋元素的方法来校正基体效应和干扰。结果:各元素在各自的检测质量浓度范围内线性关系良好(r>0.999 8),进样精密度RSD在0.8%～1.5%,重复性RSD在1.8%～6.4%,5种元素高、中、低3种浓度的加样回收率在78.9%～106.4%,样品在消解后48 h内各元素稳定性良好,铜、砷、镉、汞、铅检测下限分别为24.04、35.92、4.84、5.43、16.18 pg·mL^(-1),定量下限分别为80.13、119.72、16.13、18.10、53.94 pg·mL^(-1)。10批样品中铜含量范围为0～17.16 ng·mL^(-1),砷含量范围为6.07～11.04 ng·mL^(-1),镉含量范围为0.04～0.71 ng·mL^(-1),汞含量范围为0～1.14 ng·mL^(-1),铅含量范围为2.43～12.43 ng·mL^(-1),5种元素含量均在合格范围内。结论:本方法可用于复方苦参注射液中铜、砷、镉、汞、铅5种元素的含量测定。
Objective：To develop a method for the determination of residues of copper（Cu）, arsenic（As）, cadmium（Cd）, mercury（Hg） and lead（Pb） in compound Kushen injection.Methods：Samples were digested by microwave and measured with ICP-MS.The RF power was 1 550 W and the current velocity was 1.05 L·min^-1.Plasma gas velocity was 15.0 L·min^-1.Peristaltic pump speed was 0.2 r·s^-1 and the sampling depth was 10 mm.The signal was measured for 3 times.The internal standard solution of Ge, In and Bi were used for matrix effect correction.Results：The linearities for the elements were good with the correlation coefficients（r） being all above 0.999 8.The RSDs of the injection precision test were in the range of 0.8%-1.5% and the RSDs of the repeatability test were in the range of 1.8%-6.4%.The average recoveries of the 5 elements at three levels（high, medium and low concentration） were in the range of 78.9%-106.4%, and the digested solution was stable in 48 h.The detection limits of Cu, As, Cd, Hg and Pb were 24.04, 35.92, 4.84, 5.43 and 16.18 pg·m^L-1 and the quantitation limits were 80.13, 119.72, 16.13, 18.10, 53.94 pg·mL^-1, respectively.In 10 batches of samples, the contents of Cu, As, Cd, Hg and Pb ranged from 0 to 17.16 ng·mL^-1, 6.07 to 11.04 ng·mL-1, 0.04 to 0.71 ng·mL^-1, 0 to 1.14 ng·mL^-1 and 2.43 to 12.43 ng·mL^-1, respectively, which were all in the acceptable ranges.Conclusion：The method can be used for the content determination of Cu, As, Cd, Hg and Pb in compound Kushen injection.
作者
李耀磊
张志成
金红宇
海丽娜
韩笑
马双成
LI Yao-lei;ZHANG Zhi-cheng;JIN Hong-yu;HAI Li-na;HAN Xiao;MA Shuang-cheng(Beihua University,Jilin 132013,China;National Institutes for Food and Drug Control,Beijing 100050,China;Zhendong Pharmaceutical Research Institute Co.,Ltd.,Beijing 100085,China;Aeademy for Advaneed Interdisciplinary Studies,Peking University,Beijing 100871,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第10期1781-1787,共7页
Chinese Journal of Pharmaceutical Analysis
基金
国家十二五"重大新药创制"课题"中药质量安全检测和风险控制技术平台"(2014ZX09304307-002)
复方苦参注射液标准化建设(ZYBZH-C-JIN-43)
柴胡等9种中药饮片标准化建设(ZYBZH-C-JIN-34)
关键词
电感耦合等离子体质谱(ICP-MS)
消解
复方苦参注射液
重金属
有害元素
铅
砷
汞
镉
铜
inductively coupled plasma mass spectrometer （ ICP-MS ）
microwave digestion
compound Kushen injection
heavy metal
hazard elements
lead
arsenic
mercury
cadmium
copper
