摘要
目的:建立一种高效液相色谱联用电感耦合等离子体质谱(HPLC-ICP/MS)测定滑石粉中亚砷酸根[As(Ⅲ)]、砷酸根[As(Ⅴ)]、一甲基砷(MMA)、二甲基砷(DMA)、砷甜菜碱(AsB)和砷胆碱(AsC)共6种砷形态化合物的方法。方法:样品采用0.15 mol·L^(-1)硝酸溶液热水浴振荡提取,CNW Sep AX阴离子交换色谱柱(4 mm×250 mm,10μm),0.025 mol·L^(-1)磷酸二氢铵-水梯度洗脱,ICP-MS检测分析。结果:6种砷形态化合物在1-100μg·L^(-1)浓度范围内线性关系良好,r均>0.997;加标回收率在97.7%-99.5%之间,RSD为2.3%-4.1%(n=9)。结论:本法灵敏度高,重现性好,适用于滑石粉中6种砷形态化合物的测定,试验表明药用滑石粉中检出毒性较大的As(Ⅲ)和[As(Ⅴ)],应关注其无机砷风险。
Objective:To establish a method for the determination of six arsenic species compounds including arsenite[As(Ⅲ)],arsenate[As(Ⅴ)],monmethyl arsenic(MMA),dimethyl arsenic(DMA),arsenobetaine(AsB)and arsenocholine(AsC)in talc by high performance liqiud chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP/MS).Methods:The samples were extracted by 0.15 mol·L^(-1) nitric acid solution with water bath oscillation.A CNW Sep AX anion exchange column(4 mm×250 mm,10μm)was used with gradient elution by 0.025 mol·L^(-1) ammonium dihydrogen phosphate-water as the mobile phase,and ICP-MS was applied to the detection and analysis.Results:The linear ranges of six arsenic species compounds were between 1 and 100μg·L^(-1)with the correlation coefficients(r)above than 0.997;the average recoveries for six arsenic species compounds ranged from 97.7%to 99.5%and the RSDs ranged from 2.3%to 4.1%(n=9).Conclusion:The method is suitable for the determination of six arsenic species compounds in talc with high sensitivity and good reproducibility.As(Ⅲ)and[As(Ⅴ)]are checked out in medical talc,which is proved that inorganic arsenic risk should be concerned.
作者
陈莉
夏用恢
朱跃芳
郭沛
Chen Li;Xia Yonghui;Zhu Yuefang;Guo Pei(Zhuzhou Institute for Food and Drug Control,Hunan Zhuzhou 412000;Xiangtan Institute for Food and Drug Control)
出处
《中国药师》
CAS
2022年第6期1098-1102,共5页
China Pharmacist
