微波消解-ICP-MS测定洁白胶囊中重金属含量

Determination of the Contents of Heavy Metals in Jiebai Capsules by Microwave Digestion and ICP-MS

关键词:  电感耦合等离子体质谱法  洁白胶囊  重金属  微波消解

Key words:  ICP-MS  Jiebai capsule  heavy metals  microwave digestion

摘要:

目的 建立电感耦合等离子体质谱法（ICP-MS）测定洁白胶囊中Pb、Cd、As、Hg、Cu等重金属元素的方法，为洁白胶囊用药安全提供依据。方法 微波消解样品，以30.0 μg·L^-1的Sc 45、In 115作内标，采用ICP-MS同时测定上述5种元素的含量。结果 5种元素方法检出限为0.000 5~0.021 1 mg·kg^-1，线性关系良好（r>0.99），加样回收率为98.2%~105.4%，RSD为2.3%~3.5%。本次测定的19批洁白胶囊中重金属含量为Pb：0.2~1.0 mg·kg^-1；Cd：0.012~0.027 mg·kg^-1；As：0.18~1.52 mg·kg^-1；Hg：0~0.151 mg·kg^-1；Cu：1.4~2.5 mg·kg^-1。参照药用植物及制剂外经贸绿色行业标准和新加坡进口中药材和中成药标准，结果符合规定。结论 该方法简便易行，准确度灵敏度高、重复性良好，适用于洁白胶囊中5种重金属的测定。

Abstract:

OBJECTIVE To establish a method for determination of the contents of Pb, Cd, As, Hg, Cu in Jiebai capsule by inductively coupled plasma-mass spectrometry(ICP-MS), provide the basis for the medication safety use of Jiebai capsule. METHODS All the samples were digested by microwave, Sc 45 and In 115 of 30.0 μg·L^-1indium were used as the internal standard to determine the contents of the five elements simultaneously by ICP-MS. RESULTS The validated method indicated that correlative coefficients(r) for all elements were >0.99, and the limits of detection ranged 0.000 5-0.021 1 mg·kg^-1. The recovery rates of the method were 98.2%-105.4%, the RSD were in the range of 2.3%-3.5%. The contents of heavy metals in the 19 batches of Jiebai capsules were as follows, Pb:0.2-1.0 mg·kg^-1; Cd:0.012-0.027 mg·kg^-1; As:0.18-1.52 mg·kg^-1; Hg:0-0.151 mg·kg^-1; Cu:1.4-2.5 mg·kg^-1. Referring to foreign trade and economy green industry standards of medicinal plants and preparations and the standards of the imported Chinese medicinal herbs and Chinese patent medicine in Singapore, the results met the requirements. CONCLUSION The method is accurate, simple, sensitive and reproducible. It is suitable for the determination of the five heavy metal elements in Jiebai capsule.