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

作　　者：朱琼 方静 钱晓翠 冯璐 葛薇薇 ZHU Qiong;FANG Jing;QIAN Xiaocui;FENG Lu;GE Weiwei(Taizhou Food and Drug Inspection Institute,Taizhou,Jiangsu,China 225300)

机构地区：[1]江苏省泰州市药品检验院,江苏泰州225300

出　　处：《中国药业》2025年第8期78-81,共4页China Pharmaceuticals

基　　金：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]。

摘　　要：目的建立测定活血止痛胶囊中4种形态砷含量的高效液相色谱-原子荧光光谱联用法。方法色谱条件,色谱柱为Hamilton PRP-X100柱(250 mm×4.1 mm,10μm),流动相为12 mmol/L的磷酸氢二铵[(NH_(4))_(2)HPO_(4),用甲酸调pH至6.0],流速为1.0 mL/min,进样量为100μL,载流液为7%盐酸溶液;氢化物发生参数,还原剂为含1.5%硼氢化钾(KBH4)及0.5%氢氧化钾(KOH)的水溶液,负高压为285 V,原子化器高度为10 mm。原子荧光仪器参数,灯电流为40 mA,载气流量为300 mL/min,屏蔽器流量为800 mL/min。结果三价砷(AsⅢ)、二甲基砷(DMA)、一甲基砷(MMA)、五价砷(AsⅤ)质量浓度分别在5.060~101.2 ng/mL,5.005~101.1 ng/mL,5.020~100.4 ng/mL,5.035~100.7 ng/mL范围内与峰面积线性关系良好(r≥0.9990),检测限分别为0.088,0.131,0.119,0.381 ng/mL,定量限分别为0.290,0.432,0.357,1.143 ng/mL;精密度、稳定性、重复性试验结果的RSD均小于5%;平均加标回收率分别为95.15%,96.30%,95.58%,96.23%,RSD分别为2.87%,1.57%,2.25%,3.43%(n=9)。结论该方法操作简便,结果准确可靠,可用于测定活血止痛胶囊中4种形态砷的含量,同时为完善含砷风险高的中成药的质量标准提供技术参考。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,10μm),the mobile phase was 12 mmol/L diammonium phosphate[(NH_(4))_(2)HPO_(4),pH was adjusted to 6.0 with formic acid],the flow rate was 1.0 mL/min,the injection volume was 100μL,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≥0.9990).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 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]