莲子心饮片含量测定方法优化

Optimization of the determination method ofNelumbinis Plumula decoction pieces

为了解决提取效率低而导致的市售莲子心含量项鲜有合格的问题,对莲子心饮片中有效成分的提取方法进行优化。分别对莲心碱的提取方式、提取溶剂以及提取溶剂体积进行了考察,利用优化后的提取方法制备莲子心饮片供试品溶液,选用Kromasil 100-5-C 18(4.6 mm×150 mm)色谱柱,以乙腈-0.015 mol/L十二烷基磺酸钠溶液-冰醋酸(体积比55∶44∶1)为流动相,在流速为1.0 mL/min,柱温为30℃,检测波长为284 nm,进样量为10μL条件下,进行含量测定。结果表明,最佳的提取条件为选择25 mL 0.08%盐酸甲醇溶液作为提取溶剂,超声提取40 min;优化后的提取方法使莲心碱的含量测定较稳定,莲心碱的提取效率得到显著的提升;莲心碱进样量在36.9~369.5 ng时,线性关系良好,平均回收率为99.9%,RSD为1.79%。优化后的提取方法操作简便,提取率高,重复性好,方法准确,可为莲心碱的提取以及后续莲子心饮片质量标准的制定提供参考依据。

In order to solve the problem of the low qualification rate of content detemination items of commercial Nelumbinis Plumula decoction pieces causing by the low extraction effciency of active ingredients,the extraction method of liensinine in Nelumbinis Plumula decoction pieces was optimized.The extraction method of liensinine,the extraction solvent,and the volume of the extraction solvent were investigated respectively,and the test solution of the Nelumbinis Plumula decoction pieces was prepared by using the optimized extraction method.The method was performed on Kromasil 100-5-C 18(4.6 mm×150 mm)column with acetonitrile-0.05 mol/L sodium docecylsulfonate solution-glacial acetic acid(volume ratio 55∶44∶1)as the mobile phase.The content of liensinine in the Nelumbinis Plumula decoction pieces was determined under the conditions of the flow rate of 1.0 mL/min,the column temperature of 30°C,the detection wavelength of 284 nm,and the injection volume of 10μL.The results show that the best extraction conditions are 25 mL of 0.08%hydrochloric acid methanol solution as the extraction solvent,and ultrasonic extraction for 40 minutes.The optimized extraction method makes the content determination of liensinine more stable,and the extraction efficiency of liensinine is significantly improved.The liensinine has a good linear relationship in the injection range of 36.9~369.5 ng.The average recovery rate is 99.9%,and the RSD is 1.79%.The method is simple and accurate with the good reproducibility and high extraction rate,which can provide a reference for the extraction of liensinine and the formulation of the quality standards of Nelumbinis Plumula decoction pieces.