摘要
目的采用HPLC-MS/MS同时测定蒙药三脂清中胡椒碱、荜茇宁、柯里拉京、没食子酸、鞣花酸、槲皮素、芦丁的含量,并优化三脂清的醇提工艺。方法采用Shim-pack GIST-HP C18色谱柱(2.1 mm×100 mm,3μm),以0.1%甲酸水溶液-甲醇为流动相,梯度洗脱,流速为0.25 mL·min^(-1),进样量2μL;质谱采用电喷雾离子源,正、负离子扫描切换,多重反应监测模式进行定量分析。采用L_(9)(3^(4))正交试验设计,以上述7种成分含量的综合评分为考察指标,以料液比、乙醇浓度、提取时间、提取次数为考察因素进行三脂清醇提工艺优化。结果三脂清中7种成分的峰面积和质量浓度在一定范围内均呈现良好的线性关系(r≥0.9991),仪器精密度、重复性、稳定性试验的RSD均<5%;加样回收率为99.54%~105.32%,RSD为1.39%~4.33%。最佳醇提工艺条件为料液比1∶8,乙醇浓度40%,提取时间0.5 h,提取3次。3次放大试验验证结果显示,上述7种成分的平均含量分别为9.852,0.587,16.247,3.657,8.663,0.119,0.104 mg·g^(-1)。结论建立的方法简便、灵敏、高效,可用于三脂清中多种主要活性成分的含量测定;优化所得的醇提取工艺稳定、可行。
OBJECTIVE To develop a method for simultaneous determination of piperine,piperlonguminine,corilagin,gallic acid,ellagic acid,quercetin,rutin in Mongolian medicine Sanzhiqing by HPLC-MS/MS,and to optimize the ethanol extraction technology.METHODS The separation was performed on Shim-pack GIST-HP C18 column(2.1 mm×100 mm,3μm),mobile phase consisting of water(containing 0.1%formic acid)and methanol with gradient elution at a flow rate of 0.25 mL·min^(-1),and the injection volume was 2μL.Multiple-reaction monitoring was employed with switching electrospray ion source polarity in positive and negative mode.With comprehensive score of the content of 7 ingredients as the inspection index and material-liquid ratio,ethanol concentration,extraction time and extraction times as the inspection factor,the L_(9)(3^(4))orthogonal test design was used to optimize the ethanol extraction technology of Sanzhiqing.RESULTS There was a good linear relationship between the peak area and the mass concentration of the 7 components in Sanzhiqing(r≥0.9991).The RSD of instrument precision,repeatability and stability were all<5%,and the average recoveries ranged from 99.54%to 105.32%and the RSD ranged from 1.39%to 4.33%.The optimal ethanol extraction technology included solid-liquid ratio of 1∶8,ethanol concentration of 40%,extracting for 0.5 h and extracting for 3 times.Results of three validation tests showed that average content of the above 7 ingredients was 9.852,0.587,16.247,3.657,8.663,0.119,0.104 mg·g^(-1)respectively.CONCLUSION The established method is simple,sensitive and efficient,and can be used for determine the content of various main active ingredients in Sanzhiqing,and the optimized ethanol extraction technology is stable and feasible.
作者
胡玉霞
常福厚
李君
王跃武
张梦迪
高峰
张谦
白图雅
周树宏
HU Yuxia;CHANG Fuhou;LI Jun;WANG Yuewu;ZHANG Mengdi;GAO Feng;ZHANG Qian;BAI Tuya;ZHOU Shuhong(Inner Mongolia Medical University,the Center for New Drug Safety Evaluation and Research,Hohhot 010110,China;Inner Mongolia Medical University,Research Center for Drug Screening,Hohhot 010110,China;Inner Mongolia Medical University,College of Pharmacy,Hohhot 010110,China;Inner Mongolia Medical University,College of Basic Medicine,Hohhot 010110,China)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2022年第13期1685-1691,共7页
Chinese Journal of Modern Applied Pharmacy
基金
国家自然科学基金项目(81760676)
内蒙古自治区自然科学基金项目(2019LH08017)
内蒙古自治区高等学校科学研究项目(NJZY21593)
内蒙古医科大学实验室开放基金项目(2021LX04)
