微波辅助胶束萃取-高效液相色谱法同时测定平消片中马钱子碱、士的宁和柚皮苷的含量

Quantitative determination of brucine,strychnine and naringin in Pingxiao Tablets simultaneously by microwave-assisted micelle extraction-HPLC

目的建立一种简便快速的微波辅助胶束萃取法,用于分离测定平消片中马钱子碱、士的宁和柚皮苷的含量。方法试验以7%表面活性剂萃泽（Brij 35）为萃取溶剂,在微波功率300 W,液固比为100∶1（mL/g）的条件下,萃取2 min。分析方法采用梯度洗脱,以乙腈-0.4%磷酸水溶液（三乙胺调pH值为3.0）为流动相,检测波长为260 nm。结果马钱子碱、士的宁和柚皮苷分别在0.630~40.7、0.640~41.3、9.06~580 mg/L浓度范围内,线性关系良好（r≥0.999 3）,平均加样回收率为99.7%~101.1%,RSD为0.7%~1.0%（n=5）。结论建立的微波辅助胶束萃取法在2 min之内即可完成3种指标成分的萃取分离,大大缩短了样品前处理时间,简便快速,环境友好,结果准确可靠,为平消片生产过程中质量控制及临床药物检测提供了一种新型的、可靠的分析手段。

Objective To establish a simple and rapid microwave-assisted micelle extraction method for separate and detrmine the content of brucine,strychnine and naringin in Pingxiao Tablets.Methods The procedure was performed for 2 minutes under the conditions of 7% Brij35 as extractive solvent,300W micro power and ratio of liquid to solid as 100∶1（mL/g）.The HPLC procedure was performed in gradient elution and the mobile phase was acetonitrile-0.4% phosphoric acid solution（pH value was adjusted to 3.0 by triethylamine）.The detection wavelength was 260 nm.Results Brucine,strychnine and naringin showed a good linear relationship,respectively,at range of 0.630-40.7 mg/L,0.640-41.3 mg/L and 9.06-580 mg/L（r≥0.999 3）.The average recovery was from 99.7% to 101.1% and RSD was from 0.7% to 1.0%（n=5）.Conclusion The method established in the test can complete the extraction of the three index constituents within 2 minutes and shorten the pretreatment time,which is simple and rapid with friend environment and accurate and reliable results.It provides a new and dependable approach for quality control and clinical test of Pingxiao Tablets.