中国药业2025，Vol.34Issue(8)：78-81,4.DOI:10.3969/j.issn.1006-4931.2025.08.018
高效液相色谱-原子荧光光谱联用法测定活血止痛胶囊中4种形态砷含量
Determination of Four Forms of Arsenic in Huoxue Zhitong Capsules by High Perfor-mance Liquid Chromatography-Atomic Fluorescence Spectrometry
摘要
Abstract
Objective To establish method for the determination of four forms of arsenic in Huoxue Zhitong Capsules by high performance liquid chromatography-atomic fluorescence spectrometry.Methods The chromatographic conditions were as follows:the chromatographic column was Hamilton PRP-X100 column(250 mm×4.1 mm,10 μm),the mobile phase was 12 mmol/L diammonium phosphate[(NH4)2HPO4,pH was adjusted to 6.0 with formic acid],the flow rate was 1.0 mL/min,the injection volume was 100 μL,and the carrier liquid was 7%hydrochloric acid solution.The parameters of hydride generation were as follows:the reducing agent was an aqueous solution containing 1.5%potassium borohydride(KBH4)and 0.5%potassium hydroxide(KOH),the negative high voltage was 285 V,and the highness of atomizer was 10 mm.The atomic fluorescence instrument parameters were as follows:lamp current was 40 mA,carrier gas flow was 300 mL/min,shielding flow was 800 mL/min.Results The mass concentrations of trivalent arsenic(AsⅢ),dimethylarsenic(DMA),monomethylarsenic(MMA)and pentavalent arsenic(AsⅤ)exhibited good linear relationship with peak areas within the range of 5.060-101.2 ng/mL,5.005-101.1 ng/mL,5.020-100.4 ng/mL and 5.035-100.7 ng/mL,respectively(r≥0.999 0).The limits of detection were 0.088,0.131,0.119 and 0.381 ng/mL,respectively.The limits of quantitation were 0.290,0.432,0.357 and 1.143 ng/mL,respectively.the RSD values for precision,stability and repeatability test were less than 5%.The average spiked recovery rates were 95.15%,96.30%,95.58%and 96.23%,with RSD values were 2.87%,1.57%,2.25%,3.43%,respectively(n=9).Conclusion This method is simple,accurate and reliable,which can be used to determine the content of four forms of arsenic in Huoxue Zhitong Capsules,and provide technical reference for improving the quality standard of Chinese patent medicines with high risk of arsenic.关键词
活血止痛胶囊/高效液相色谱法/原子荧光光谱法/砷形态/含量测定Key words
Huoxue Zhitong Capsule/high performance liquid chromatography/atomic fluorescence spectrometry/arsenic speciation/content determination分类
医药卫生引用本文复制引用
朱琼,方静,钱晓翠,冯璐,葛薇薇..高效液相色谱-原子荧光光谱联用法测定活血止痛胶囊中4种形态砷含量[J].中国药业,2025,34(8):78-81,4.基金项目
国家药品监督管理局化学药品杂质谱研究重点实验室开放研究课题[NMPA-KLIPCD-2023-06]. （）
