高效液相色谱法快速检测商陆中毒样品中的两种商陆皂苷

Rapid determination of 2 kinds of esculentoside in Radix Phytolaccae poisoning samples by high performance liquid chromatography

目的建立高效液相色谱法快速检测商陆中毒样品中商陆皂苷的方法。方法采用微波辅助萃取法,提取商陆中的商陆皂苷甲和商陆皂苷乙,C18色谱柱分离后,采用紫外检测器进行测定,检测波长203nm,流动相为乙腈-0.01%磷酸溶液,流速为1.0mL/min。结果商陆皂苷甲和商陆皂苷乙在质量浓度0~500μg/mL范围内呈良好线性关系,相关系数均>0.999,检出限分别为36.5、96.5mg/kg。加标回收率为96.3%~98.6%,相对标准偏差(RSD)为0.13%~0.54%。结论建立的方法简单、快速、准确,适用于商陆中毒样品中两种商陆皂苷的应急检测需要。

Objective To establish a method for the determination of esculentoside in poisoning Radix Phytolaccae samples by high performance liquid chromatography(HPLC).Methods The esculentoside A and esculentoside B in the Radix Phytolaccae samples were extracted by microwave-assisted extraction.The separation was performed on C18 column using acetonitrile-0.01%phosphate acid as the mobile phase at a flow rate of 1.0 mL/min.The ultraviolet analyte was used for detection at wavelength of 203 nm.Results Both esculentoside A and esculentoside B showed good linear relationship in the range of 0-500μg/mL with the correlation coefficient greater than 0.999,the limit of detections were 36.5 mg/kg and 96.5 mg/kg,respectively.The spiked recoveries were 96.3%-98.6%,with the relative standard deviation(RSD)of 0.13%-0.54%.Conclusions The established method is simple,rapid and accurate,which can satisfy the requirements for emergency simultaneous determination of esculentoside A and B in poisoning Radix Phytolaccae.