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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 micellar extraction method for the determination of brucine, strychnine and naringin in Pingdu Tablet. Methods The experiment was carried out with Brij 35 as extracting solvent and extraction for 2 min under microwave power of 300 W and liquid / solid ratio of 100:1 (mL / g). The analytical method was gradient elution. The mobile phase consisted of acetonitrile-0.4% phosphoric acid (adjusted to pH 3.0 with triethylamine) and the detection wavelength was 260 nm. Results The contents of strychnine, strychnine and naringin were good linearity (r≥0.999 3) in the range of 0.630 ~ 40.7,0.640 ~ 41.3 and 9.06 ~ 580 mg / L, respectively. The average recoveries were 99.7% % ~ 101.1%, RSD 0.7% ~ 1.0% (n = 5). Conclusion The established microwave-assisted micellar extraction method can complete the extraction and separation of three kinds of index components within 2 minutes, greatly shortening the sample pretreatment time, being simple and rapid, environment-friendly and accurate and reliable. Quality control and clinical drug testing provide a new, reliable analytical tool.