摘要
目的：应用电感耦合等离子体质谱技术（ICP-MS）建立同时测定清开灵系列制剂（注射液、软胶囊、胶囊、颗粒）中锂、铍、硼、钒、铬、钴、镍、铜、镓、砷、硒、镉、锑、钡、汞、铊、铅17种元素的方法。方法：清开灵系列制剂（胶囊20批,颗粒30批,软胶囊6批,注射液39批）经微波消解后采用ICP-MS测定,射频（RF）入射功率为1.3 k W,采样深度为65 mm,冷却气、辅助气和载气流量分别为13.0、0.81和0.80 L·min-1,积分时间为0.5~2 s。通过在线加入内标锗、铟、铼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均不低于0.999 1）,检出限为0.005~0.502 ng·m L-1,不同剂型中各元素的回收率为85.4%~110.7%,RSD为0.4%~5.2%,仪器精密度RSD〈3%,稳定性RSD〈5%。参照中国药典2010年版第二增补本,各批样品中重金属及有害元素铅、镉、砷、汞、铜的含量基本在合格范围内。结论：该方法简便、灵敏、准确,可用于清开灵系列制剂中多种元素的检测,为其风险监控提供了技术参数。
Objective： To establish a method for the content determination of 17 elements such as Li,Be,B,V,Cr, Co,Ni,Cu,Ga,As,Sr, Cd, Sb, Ba, Hg,T1,Pb in Qingkailing preparations, including injections, capsules, soft capsules and granules by inductively coupled plasma mass spectrometry （ ICP- MS）. Methods： Totally 20 batches of capsules, 30 batches of granules,6 batches of soft capsules and 39 batches of injections were collected. Samples were digested by microwave and measured with ICP-MS. The RF power was 1.3 kW,and the sampling depth was 65 mm. The flow rate of plasma gas, auxiliary gas and carrier gas were 13.0 L ·min-1,0. 81 L · min-1 and 0. 80 L·min-1 ,respectively. The integration time was 0. 5 -2 s. The internal standard solution with Ge, In and Re were used to help avoid the interference of matrix elements and spectra. Results： The validated method indicated that the linearity was good and the correlative coefficients（r）for elements were all above 0. 999 1. The limits of detections were in the range of 0. 005 to 0. 502 ng· mL-1. The recoveries of elements were between 85.4% and 110. 7% with RSD 0. 4% to 5.2%. The precision and stability were good with RSD less than 3% and 5% respectively. The contents of heavy metals and hazard elements such as Pb, Cd, As, Hg, Cu in samples were basically within the designated range according to China Pharmacopoeia 2010 Supplement I1. Conclusion： The method is simple, sensitive and accurate, and it can be used for the content determination of multiple elements in Qingkailing preparations, providing helpful information for the risk monitoring.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第11期2018-2023,共6页
Chinese Journal of Pharmaceutical Analysis
基金
国家自然科学基金青年科学基金(81302654)
