温肾健脾定脊合剂指标成分测定及水提工艺研究  

Determination of Indicator Components and Optimization of Water Extraction Process of Wenshen Jianpi Dingji Mixture

作　　者：钱芳[1] 何晓瑾[1,2] 杨秀珍[1] QIAN Fang;HE Xiaojin;YANG Xiuzhen(Jiangsu Provincial Hospital of Traditional Chinese Medicine,Nanjing,Jiangsu,China 210029;The First Clinical Medical College,Nanjing University of Chinese Medicine,Nanjing,Jiangsu,China 210023)

机构地区：[1]江苏省中医院,江苏南京210029 [2]南京中医药大学第一临床医学院,江苏南京210023

出　　处：《中国药业》2024年第22期64-68,共5页China Pharmaceuticals

基　　金：江苏省科技项目[BE2022801];江苏省中医院科技项目[Y2020CX54]。

摘　　要：目的优选温肾健脾定脊合剂水提工艺。方法采用高效液相色谱-蒸发光散射检测器(HPLC-ELSD)法测定耐斯糖含量,采用高效液相色谱-二极管阵列检测器(HPLC-DAD)法测定芍药苷、升麻素苷、5-O-甲基维斯阿米醇苷和柚皮苷的含量。以加水量、提取时间、提取次数为考察因素,以上述指标成分总量及干膏得率为评价指标,采用L_(9)(3^(4))正交试验优选水提工艺,并验证。结果耐斯糖、芍药苷、升麻素苷、5-O-甲基维斯阿米醇苷和柚皮苷的进样量分别在1.054~10.54μg(r=0.9998)、0.8076~10.768μg(r=0.9999)、0.1383~1.844μg(r=0.9999)、0.1917~2.556μg(r=1.0000)、0.4803~6.404μg(r=0.9999)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为97.79%,100.73%,98.56%,101.38%,97.31%,RSD分别为1.74%,1.49%,1.34%,2.05%,1.66%(n=9)。最优水提工艺为加8倍量水,提取2次,每次40 min。结论所建立的指标成分含量测定方法及优选的水提工艺稳定、可行,可为温肾健脾定脊合剂的进一步开发提供参考。Objective To optimize the water extraction process of Wenshen Jianpi Dingji Mixture.Methods The high-performance liquid chromatography-evaporative light scattering detection(HPLC-ELSD)was used to determine the content of nystose,and the high-performance liquid chromatography-diode array detector(HPLC-DAD)was used to determine the contents of paeoniflorin,prim-O-glucosylcimifugin,5-O-methylvisammioside and naringin.The L_(9)(3^(4))orthogonal test was used to optimize the water extraction process with the water addition amount,extraction time and extraction frequency as the investigation factors,and with the total amount of the above indicator components and yield of dry extract as the evaluation indicators,and the verification test was carried out.Results The linear ranges of nystose,paeoniflorin,prim-O-glucosylcimifugin,5-O-methylvisammioside and naringin were 1.054-10.54μg(r=0.9998),0.8076-10.768μg(r=0.9999),0.1383-1.844μg(r=0.9999),0.1917-2.556μg(r=1.0000),0.4803-6.404μg(r=0.9999),respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rates of the above five components were 97.79%,100.73%,98.56%,101.38%,97.31%,with RSDs of 1.74%,1.49%,1.3~4%,2.05%,1.66%(n=9)respectively.The optimal water extraction process was as follows:adding eight times the amount of water,extracting twice,each time for 40 min.Conclusion The established content determination method of indicator components and the optimal water extraction process are stable and feasible,which can provide a reference for the further development of Wenshen Jianpi Dingji Mixture.

关 键 词：温肾健脾定脊合剂 正交试验 提取工艺 耐斯糖 芍药苷 升麻素苷 5-O-甲基维斯阿米醇苷 柚皮苷 含量测定 

分 类 号：R943[医药卫生—药剂学]