基于HPLC联合ICP-MS法测定活血止痛胶囊中总砷、可溶性砷、价态砷

Determination of Total Arsenic, Soluble Arsenic and Valent Arsenic in Blood Huoxue Zhitong Capsules by High Performance Liquid Chromatography Combined with ICP-MS

目的:测定活血止痛胶囊中总砷、可溶性砷及价态砷含量。方法:采用微波消解法联合电感耦合等离子体质谱(ICP-MS)测定活血止痛胶囊总砷量,同时用人工胃液、人工肠液处理样品,以ICP-MS和高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分别测定可溶性砷及价态砷。结果:7批样品不同厂家间总砷量相差较大;经人工胃液和肠液分别提取后测得的可溶性砷含量,人工胃液>人工肠液;6种价态砷均仅检出三价砷As(Ⅲ),各批三价砷测得量占可溶性砷的比例,人工肠液>人工胃液。结论:控制含砷风险高的中成药质量,测定可溶性砷及砷价态含量比单纯制定总砷标准更为科学合理,活血止痛胶囊中可溶性砷和价态砷明显低于总砷量,该方法准确、重复性好,为评价活血止痛胶囊的安全性提供参考。

Objective:To determine total arsenic,soluble arsenic and valent arsenic in huoxue zhitong capsules.Method:The content of total arsenic in blood huoxue zhitong capsules was determined by microwave digestion combined with inductively coupled plasma mass spectrometry(ICP-MS).The samples were treated with artificial gastric juice and artificial intestinal juice,and the contents of soluble arsenic and valent arsenic were determined by ICP-MS and high performance liquid chromatography-inductively coupled plasma(HPLC-ICPMS).Results:The content of total arsenic in seven batches of samples from different manufacturers varied greatly.The content of soluble arsenic measured after extraction with arti?cial gastric juice was higher than that measured after extraction with arti?cial intestinal juice.Only trivalent arsenic(Ⅲ)(As3+)was detected in all six kinds of valent arsenic,and the ratio of trivalent arsenic to soluble arsenic in each batch of samples was in order of arti?cial intestinal?uid>arti?cial gastric juice.Conclusion:It is more scienti?c and reasonable to control the quality of Chinese patent medicines with high risk of arsenic and to determine the content of soluble arsenic and valent arsenic than to establish the total arsenic standards alone.The contents of soluble arsenic and valent arsenic in huoxue zhitong capsules are signi?cantly lower than the content of total arsenic.The method is accurate and reproducible,and provides a reference for evaluating the safety of blood circulation-promoting and pain-relieving capsules.