摘要
目的建立同时测定桂附地黄丸(浓缩丸)中5种成分含量的方法。方法采用高效液相色谱(HPLC)法测定样品含量。色谱柱为Welch Ultimate XB-C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长为236 nm(莫诺苷、马钱苷、芍药苷)、290 nm(桂皮醛、丹皮酚),进样量为10μL,柱温为35℃。并对样品含量进行聚类分析。结果桂皮醛、丹皮酚、芍药苷、莫诺苷、马钱苷质量浓度分别在0.49~24.44μg/mL(r=0.9997)、11.11~555.44μg/mL(r=0.9999)、4.53~226.51μg/mL(r=0.9997)、6.99~349.52μg/mL(r=0.9999)、6.34~317.04μg/mL(r=0.9996)范围内与峰面积线性关系良好(n=6),定量限分别为0.17,0.39,0.51,1.10,0.58μg/mL;精密度、稳定性、重复性试验结果的RSD均小于2%;平均加样回收率为96.69%,98.19%,99.37%,97.50%,98.09%,RSD分别为1.53%,0.74%,1.99%,2.11%,1.75%(n=6)。21批次样品聚类分为6类。结论该方法操作简便、结果准确,符合测定要求,可用于同时测定桂附地黄丸(浓缩丸)中5种成分含量。
Objective To establish a method for simultaneous determination of five components in Guifu Dihuang Pills(concentrated pills).Methods The sample content was determined by high-performance liquid chromatography(HPLC).The column was Welch Ultimate XB-C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.1% phosphoric acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 236 nm(morroniside,loganin,paeoniflorin)and 290 nm(cinnamaldehyde,paeonol),the injection volume was 10μL,and the column temperature was 35°C.The samples were analyzed by cluster analysis.Results Cinnamaldehyde,paeonol,paeoniflorin,morroniside,and loganin showed good linear relationships with peak areas within the ranges of 0.49-24.44μg/mL(r=0.9997),11.11-555.44μg/mL(r=0.9999),4.53-226.51μg/mL(r=0.9997),6.99-349.52μg/mL(r=0.9999),and 6.34-317.04μg/mL(r=0.9996)(n=6),respectively.The limits of quantification were 0.17,0.39,0.51,1.10,and 0.58μg/mL,respectively.The RSDs of precision,stability,and repeatability tests were all less than 2%.The average recoveries were 96.69%,98.19%,99.37%,97.50%,and 98.09%,and the RSD were 1.53%,0.74%,1.99%,2.11%,and 1.75%(n=6),respectively.Cluster analysis classified the 21 batches of samples into six categories.Conclusion This method is simple,accurate,and can meet the requirements for simultaneous determination of the five components in Guifu Dihuang Pills(concentrated pills).
作者
孙迎春
刘喜
刘东风
潘竹青
SUN Yingchun;LIU Xi;LIU Dongfeng;PAN Zhuqing(Food and Drug Inspection Center of Anqing,Anqing,Anhui,China 246001)
出处
《中国药业》
2025年第8期74-78,共5页
China Pharmaceuticals
基金
安徽省药品监督管理局科技创新项目[AHYJ-KJ-202321]。
作者简介
第一作者:孙迎春,女,大学本科,副主任中药师,研究方向为中药检验及质量控制,(电子信箱)xuanqi2009@126.com。
