摘要
探讨甘露饮中6种有效成分(绿原酸、麦角甾苷、柚皮苷、黄芩苷、甘草酸、熊果酸)最佳提取工艺条件及含量测定方法。优化提取溶剂,通过正交试验法考察料液比、提取时间和提取次数对甘露饮提取工艺的影响。采用Syncronis C18色谱柱(4.6mm×250mm,5μm),流动相乙腈(A)-0.1%磷酸水溶液(B)梯度洗脱(0~5min,5%A;5~40min,5%~20%A;40~60min,20%~50%A;60~80min,50%~90%A;80~90.1min,90%~5%A;90.1~100min,5%A),流量1.0mL/min,柱温35℃,检测波长210nm,进样量20μL的色谱条件对甘露饮提取物中6种有效成分进行含量测定。最佳提取工艺条件是:60%乙醇为提取溶剂,料液比1∶4,提取时间为1h,提取次数为1次。绿原酸、麦角甾苷、柚皮苷、黄芩苷、甘草酸、熊果酸分别在4.80~80.00,10.00~100.00,24.00~400.00,30.00~500.00,6.00~100.00,3.60~60.00μg/mL浓度范围内线性关系良好(r^2≥0.9995)。平均加样回收率在96.12%~101.82%,RSD在1.72%~2.92%。该提取工艺稳定可行,HPLC法能简便、准确地测定甘露饮提取物中6种有效成分的含量。
To investigate the optimum extraction condition and content determination of six effective components (chlorogenic acid, acteoside, naringin, baicalin, glycyrrhizic acid, ursolic acid) in Ganlu Yin. Extraction solvent was optimized, the effects of the amount of solid-liquid ratio, extraction time and extraction times on the extraction technology of Ganlu Yin were investigated by orthogonal test. Six effective components in the Ganlu Yin extracts were determined on Syncronis C18 column (4.6 mm×250 mm, 5 μm), and eluted with the mobile phase of acetonitrile (A) and 0.1% phosphoric acid (B) with linear gradient mode (0-5 min, 5% A;5-40 min, 5%-20% A;40-60 min, 20%-50% A;60-80 min, 50%-90% A;80-90.1 min, 90%- 5% A;90.1-100 min, 5% A), the flow rate of the mobile phase was 1.0 mL/min with the column temperature of 35 ℃, and the detection wavelengths were at 210 nm,and the sample size of 20 μL . The optimum extraction process was as follows: 60% ethanol as extraction solvent, solid-liquid ratio 1∶4, 1h for each time and extracting one time. The linea ranges of chlorogenic acid, acteoside, naringin, baicalin, glycyrrhizic acid and ursolic acid was 4.80-80.00, 10.00-100.00, 24.00-400.00, 30.00-500.00, 6.00-100.00, 3.60-60.00 μg/mL (r^2≥0.999 5), respectively. The mean recoveries were 96.12%-101.82% with RSD between 1.72%~2.92%.This extraction process is stable and feasible, and the six effective components in Ganlu Yin extracts can be determined simply and accurately by HPLC.
作者
黄亚
宿怀予
范秀
周荣
廖昌军
HUANG Ya;SU Huaiyu;FAN Xiu;ZHOU Rong;LIAO Changjun(Deyang People’s Hospital in Sichuan Province,Deyang 618000,China;School of Pharmacy,Chengdu Medical College,Chengdu 610083,China)
出处
《中国测试》
CAS
北大核心
2019年第6期81-87,共7页
China Measurement & Test
基金
德阳市科技局支撑计划(2016SZ033)