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正交试验优选栀子的水提醇沉工艺
引用本文:毕宏生,郭俊国,解孝锋.正交试验优选栀子的水提醇沉工艺[J].中国实验方剂学杂志,2014,20(1):19-23.
作者姓名:毕宏生  郭俊国  解孝锋
作者单位:山东中医药大学眼科研究所, 济南 250002;山东中医药大学附属眼科医院, 济南 250002;山东中医药大学眼科研究所, 济南 250002;山东省中西医结合眼病防治重点实验室, 济南 250002;山东中医药大学附属眼科医院, 济南 250002
基金项目:国家自然科学基金项目(81072961)
摘    要:目的:优选栀子的水提醇沉工艺。方法:采用HPLC-DAD在238,440 nm处检测特征峰,以栀子苷峰面积和HPLC指纹图谱确定的14个化学成分峰面积之和为综合评价指标,通过正交试验设计,考察加水量、煎煮时间和煎煮次数对栀子水提工艺的影响,考察提取液相对密度、醇沉浓度、搅拌速度和醇沉时间对栀子水提液醇沉工艺的影响。结果:在238,440 nm处分别确定了栀子中10,4个化学成分的特征图谱。最佳水提工艺为加10倍量水煎煮3次,每次30 min;最佳醇沉工艺为醇沉浓度70%,药液初始相对密度1.10 g·mL-1,搅拌速度200 r·min-1,醇沉时间10 h。结论:采用已知、未知结构成分HPLC指纹图谱相结合的方法优选的工艺准确性更高,为中药提取工艺的研究提供参考。

关 键 词:栀子  高效液相色谱  指纹图谱  栀子苷  正交试验  水提醇沉工艺
收稿时间:2013/5/14 0:00:00

Optimization of Water Extraction and Alcohol Precipitation Process for Gardeniae Fructus by Orthogonal Design
BI Hong-sheng,GUO Jun-guo and XIE Xiao-feng.Optimization of Water Extraction and Alcohol Precipitation Process for Gardeniae Fructus by Orthogonal Design[J].China Journal of Experimental Traditional Medical Formulae,2014,20(1):19-23.
Authors:BI Hong-sheng  GUO Jun-guo and XIE Xiao-feng
Institution:Eye Institute of Shandong University of Traditional Chinese Medicine(TCM), Ji'nan 250002, China;Eye Hospital Affiliated Shandong University of TCM, Ji'nan 250002, China;Eye Institute of Shandong University of Traditional Chinese Medicine(TCM), Ji'nan 250002, China;Shandong Provincial Key Laboratory of Integrated Traditional Chinese and Western Medicine for Prevention and Therapy of Ocular Diseases, Ji'nan 250002, China;Eye Hospital Affiliated Shandong University of TCM, Ji'nan 250002, China
Abstract:Objective: To optimize water extraction and alcohol precipitation process of Gardeniae Fructus. Method: Characteristic peaks were detected at 238 and 440 nm by HPLC-DAD,with peak area of geniposide and total peak areas of fourteen chemical ingredients identified by HPLC fingerprint as comprehensive evaluation index,orthogonal test was adopted to optimize water extraction technology of Gardeniae Fructus by taking the amount of water,decocting time and decocting times as factors;Effects of relative density of extract,alcohol precipitation concentration,stirring speed and alcohol sedimentation time on alcohol precipitation process of water extract were investigated by orthogonal test. Result: Ten and four characteristic peaks in Gardeniae Fructus were determined at 238 and 440 nm,respectively.The best water extraction was as following:decocted three times with ten times the amount of water,30 min each time;Optimum alcohol precipitation process was:relative density of water extract 1.10 g·mL-1,alcohol precipitation concentration 70%,stirring speed 200 r·min-1,alcohol sedimentation time for 10 h. Conclusion: These processes had high accuracy which were optimized by combining with HPLC fingerprints of known and unknown structural components,this study could provide a reference for optimizing extraction technology of traditional Chinese medicine.
Keywords:Gardeniae Fructus  HPLC  fingerprint  geniposide  orthogonal test  water extraction and alcohol precipitation technology
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