高效液相色谱-电感耦合等离子体质谱法测定接骨七厘片中总砷含量及砷形态分析  

Analysis of Total Arsenic Content and Arsenic Species in Jiegu Qili Tablets by HPLC-ICP-MS

作　　者：朱琼 方静 蔡鹏[1] 钱保勇[1] ZHU Qiong;FANG Jing;CAI Peng;QIAN Baoyong(Taizhou Institute for Food and Drug Control,Taizhou,Jiangsu,China)

机构地区：[1]江苏省泰州市食品药品检验所,江苏泰州225300

出　　处：《中国药业》2020年第15期78-81,共4页China Pharmaceuticals

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.

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 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学]