摘要
目的:探讨不同产地丹参中总砷及砷形态的含量测定方法,为丹参药材的评价积累数据,同时为含有丹参的中药制剂的风险防控提供数据支持。方法:采用电感耦合等离子体质谱法(ICP-MS)测定不同产地丹参中总砷的含量;采用高效液相色谱-电感耦合等离子体质谱联用法(HPLC-ICP-MS)测定不同产地丹参中6种砷形态的含量。结果:总砷在2.0~20 ng·mL^-1范围内线性关系良好,标准曲线相关系数r=0.9992,检测限(LOD)=0.0016 ng·mL^-1,加标回收率为98.3%~99.2%,RSD<3.7%(n=3);六种砷形态在2.0~20 ng·mL^-1范围内线性关系良好,标准曲线的相关系数r均>0.999,检测限(LOD)在0.0029~0.0103 ng·mL^-1之间,加标回收率为89.6%~95.9%,RSD<7.7%(n=3)。采用HPLC-ICP-MS测定了不同产地丹参中六种砷形态的含量,结果表明丹参中含有少量AsB、As(Ⅲ),As(Ⅴ),各产地丹参中的总砷含量虽然高,但是有毒的砷形态含量较低。结论:本法经初步方法学验证,可用于中药材及制剂中的砷含量的测定。
Objective:To explore the test method of total arsenic and arsenic species analysis in Radix et Rhizoma from the different origins,to accumulate the data for the evaluation of Radix et Rhizoma and to provide the data support for risk control of traditional medicines preparations.Methods:Inductively coupled plasma mass spectrometry(ICP-MS)method was used to determine the contents of total arsenic in Radix et Rhizoma.High performance liquid chromatography-Inductively Coupled Plasma Mass Spectrometry(HPLC-ICP-MS)method was used to determine six arsenic species in Radix et Rhizoma from the different origins.Results:The linear range of total arsenic fell into 2.0-20 ng·mL^-1 with r as 0.9992.The limit of detection(LOD)was 0.0016 ng·mL^-1 and the recoveries were 98.3%-99.2%with RSD<3.7%(n=3).The linear range of six arsenic species fell into 2.0-20 ng·mL^-1 with r>0.999.The limits of detection(LOD)were 0.0029-0.0103 ng·mL^-1,and the spiked recoveries were 89.6%-95.9%with RSD<7.7%(n=3).The contents of six arsenic species in Radix et Rhizoma from the different origins were determined by HPLC-ICP-MS.The test results showed that the less contents of AsB,As(Ⅲ),As(Ⅴ)was found in Salvia miltiorrhiza Bunge.Although the content of total arsenic in Salvia miltiorrhiza Bunge was high,that of toxic arsenic species was lower.Conclusion:This established method has been preliminarily validated and it can be utilized for determination of arsenic species in Chinese herbal medicines and preparations.
作者
柏大为
朱琼
BO Dawei;ZHU Qiong(Taizhou Institute for Food and Drug Control,Taizhou 225300,China)
出处
《中国药品标准》
CAS
2019年第6期526-531,共6页
Drug Standards of China
