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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 simultaneous determination of lithium, beryllium, boron, vanadium, chromium, cobalt, nickel, copper, calcium and magnesium in Qingkailing preparations (injection, soft capsule, capsule and granule) by inductively coupled plasma mass spectrometry (ICP- Gallium, arsenic, selenium, cadmium, antimony, barium, mercury, thallium, lead 17 kinds of elements of the method. Methods: The content of radio frequency (RF) incidental power was determined by ICP-MS after microwave digestion. The sampling power of Qingkailing series was 20 kDa, 30 batches, 6 batches of soft capsule and 39 batches of injection. 65 mm, the cooling gas, auxiliary gas and carrier gas flow rate were 13.0,0.81 and 0.80 L · min-1, the integration time is 0.5 ~ 2 s. The matrix effects and interferences are corrected by the online addition of the germanium, indium and rhenium elements. Results: The results showed that the linearity of each element was good (r less than 0.999 1) and the limit of detection was 0.005-0.502 ng · m L-1. The recovery rate of each element in different dosage forms was 85.4% ~ 110.7%, RSD 0.4% -5.2%, RSD <3%, RSD <5%. Reference to the Chinese Pharmacopoeia 2010 edition of the second supplement, the samples of heavy metals and harmful elements lead, cadmium, arsenic, mercury, copper content basically within the eligible range. Conclusion: The method is simple, sensitive and accurate and can be used for the detection of a variety of elements in Qingkailing series preparations, providing technical parameters for risk monitoring.