摘要
目的建立测定接骨七厘片中总砷含量的电感耦合等离子体质谱(ICP-MS)法,以及测定砷形态含量的高效液相色谱仪-电感耦合等离子体质谱联用(HPLC-ICP-MS)法。方法采用ICP-MS法测定接骨七厘片中总砷的含量;采用HPLC-ICP-MS法测定接骨七厘片中砷甜菜碱(AsB)、砷胆碱(As C)、一甲基砷(MMA)、二甲基砷(DMA)、亚砷酸盐As(Ⅲ)、砷酸盐As(Ⅴ)的含量。结果总砷质量浓度线性范围是2.0~20.0 ng/m L(r=0.9992);检测限为0.0016 ng/m L;加样回收率为98.23%~99.95%,RSD小于3.25%(n=3);As B,As C,MMA,DMA,As(Ⅲ),As(Ⅴ)6种砷形态线性关系均良好(r>0.999),检测限范围为0.0029~0.0103 ng/m L,加样回收率为89.15%~95.89%,RSD小于7.14%(n=3)。接骨七厘片中含有MMA,DMA,As(Ⅲ),As(Ⅴ),其中As(Ⅴ)含量最高,其次是As(Ⅲ),以及少量的MMA和DMA。结论该方法经方法学验证,可用于中药材及制剂中砷含量的测定。
Objective To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of total arsenic content in Jiegu Qili Tablets,and a high performance liquid chromatograph-inductively coupled plasma mass spectrometry(HPLC-ICP-MS)method for the determination of arsenic species.Methods The ICP-MS method was used to determine the total arsenic content in Jiegu Qili Tablets.The HPLC-ICP-MS method was used to determine the contents of arsenic betaine(ASB),arsenic choline(ASC),and monomethyl arsenic(MMA),Dimethyl arsenic(DMA),arsenite As(Ⅲ),arsenate As(Ⅴ)in Jiegu Qili Tablets.Results Total arsenic showed good linear relationship in the range of 2.0-20.0 ng/m L(r=0.9992);the detection limit was 0.0016 ng/m L,the recovery was 98.23%-99.95%,and the RSD was less than 3.25%(n=3);the 6 kinds of arsenic species AsB,As C,MMA,DMA,As(Ⅲ),As(Ⅴ)all showed good linear relationship(r>0.999);the detection limit was 0.0029-0.0103 ng/m L,the recoveries was89.15%-95.89%,the RSD was less than 7.14%(n=3).There were MMA,DMA,As(Ⅲ),and As(Ⅴ)in the Jiegu Qili Tablets,and As(V)had the highest content,followed by As(Ⅲ),and a small amount of MMA and DMA.Conclusion This method has been preliminary validated and can be utilized for the test of arsenic species in Chinese herbal medicines and preparations.
作者
朱琼
方静
蔡鹏
钱保勇
ZHU Qiong;FANG Jing;CAI Peng;QIAN Baoyong(Taizhou Institute for Food and Drug Control,Taizhou,Jiangsu,China)
出处
《中国药业》
CAS
2020年第15期78-81,共4页
China Pharmaceuticals
关键词
高效液相色谱-电感耦合等离子体质谱联用法
接骨七厘片
砷形态
含量测定
high performance liquid chromatograph-inductively coupled plasma mass spectrometry
Jiegu Qili Tablets
arsenic species
content determinations
