夏天一,张凤,韩强,习峰敏,高守红,殷军,陈万生
XIA Tian-yi,ZHANG Feng,HAN Qiang,XI Feng-min,GAO Shou-hong,YIN Jun,CHEN Wan-sheng

• 1:上海长征医院药学部
• 2:沈阳药科大学中药学院

摘要(Abstract)：

目的建立同时测定墨旱莲药材中蟛蜞菊内酯、旱莲苷Ⅰ和旱莲苷Ⅶ含量的方法。方法采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD)。色谱柱为Agilent Zorbax SB-C18柱(250 mm×4.6 mm,5μm);流动相为乙腈和体积分数为0.5%甲酸水溶液,采用梯度洗脱程序;流速为1.0 m L·min-1;柱温为25℃;进样量为20μL。蒸发光散射检测器漂移管温度为40℃,载气压力为4.0bar。结果蟛蜞菊内酯、旱莲苷Ⅰ和旱莲苷Ⅶ分别在质量浓度为5.120~51.15 mg·L~(-1)、5.100~50.95 mg·L~(-1)和1.970~19.74 mg·L~(-1)内与峰面积呈良好的线性关系;重复性好(RSD<2.1%),中间精密度佳(RSD<1.8%),准确度分别为99.81%(RSD=1.4%)、97.52%(RSD=2.3%)和99.74%(RSD=1.5%)。结论该方法可作为控制墨旱莲质量的标准之一。
Objective To establish a method for simultaneous quantification of wedelolactone,eclalbasaponin I and eclalbasaponin VII in Eclipta prostrata.Methods HPLC-ELSD was applied and separation was carried out on an Agilent Zorbax SB-C18column(250 mm × 4.6 mm,5 μm) using mobile phase of acetonitrile and0.5% formic acid(φ) aqueous solution in gradient elution at a flowspeed of 1.0 m L·min- 1.The column temperature was set at 25 ℃ and the injection volume was 20 μL.For setting of ELSD,the drift tube temperature was set at 40 ℃ and the carrier gas pressure was 4.0 bar.Results Good calibration linearity was achieved for wedelolactone,eclalbasaponin I and eclalbasaponin VII in the range of 5.120- 51.15 mg·L~(-1),5.100- 50.95 mg·L~(-1)and 1.970- 19.74 mg·L~(-1),respectively.The repeatability was good with RSDs <2.1%,and the RSDs of intermediate precision were < 1.8%.Accuracy was 99.81%(RSD = 1.4%) for wedelolactone,97.52%(RSD = 2.3%) for eclalbasaponin I,and 99.74%(RSD = 1.5%) for eclalbasaponin VII.Conclusions The established method is simple and feasible for the simultaneous determination of wedelolactone,eclalbasaponin I and eclalbasaponin VII,which provides references for the quality control of Eclipta prostrate.

关键词(KeyWords)： 墨旱莲;高效液相色谱;蟛蜞菊内酯;旱莲苷Ⅰ;旱莲苷Ⅶ;含量
Eclipta prostrate;HPLC;wedelolactone;eclalbasaponin Ⅰ;eclalbasaponin Ⅵ;concentration

Abstract:

Keywords:

基金项目(Foundation): “重大新药创制”国家科技重大专项资助项目(2013ZX09507005)

作者(Author): 夏天一,张凤,韩强,习峰敏,高守红,殷军,陈万生
XIA Tian-yi,ZHANG Feng,HAN Qiang,XI Feng-min,GAO Shou-hong,YIN Jun,CHEN Wan-sheng

DOI: 10.14066/j.cnki.cn21-1349/r.2017.01.011

参考文献(References)：

• [1]任笑传,程凤银.墨旱莲的化学成分、药理作用及其临床应用[J].解放军预防医学杂志,2013,31(6):559-561.
• [2]李娟,王玉香.墨旱莲化学成分及药理作用研究概况[J].中国药师,2010,13(8):1193-1194.
• [3]营大礼.墨旱莲化学成分、药理作用及临床应用研究进展[J].中国药房,2008,19(36):2876-2878.
• [4]原红霞,赵云丽,闫艳,等.墨旱莲的化学成分[J].中国实验方剂学杂志,2011,17(16):103-105.
• [5]施嫣嫣,张丽,丁安伟.墨旱莲化学成分及药理作用研究[J].吉林中医药,2011,31(1):68-70.
• [6]吴疆,侯文彬,张铁军.墨旱莲的化学成分研究[J].中草药,2008,39(6):814-816.
• [7]李春洋,白秀珍,程静.墨旱莲全草、茎、叶提取液对肝保护作用的研究[J].数理医药学杂志,2005,18(6):586-588.
• [8]欧阳蒲月,梁永枢,莫小路,等.墨旱莲提取物抑菌活性初步研究[J].亚热带植物科学,2013,42(3):199-204.
• [9]刘翔,陈晓风,栾雨.不同产地墨旱莲中总黄酮含量测定比较[J].江苏中医药,2007,39(10):65-66.
• [10]陈腾飞,萧伟,尚强,等.HPLC法测定不同产地墨旱莲药材中木犀草素含量[J].南京中医药大学学报,2011,27(2):158-160.
• [11]FANG X S,WANG J H,HAO J F,et al.Simultaneous extraction,identification and quantification of phenolic compounds in Eclipta prostrata using microwave-assisted extraction combined with HPLC-DAD-ESI-MS/MS[J].Food Chemistry,2015,188:527-536.
• [12]周燕园,吴怀恩,梁臣艳,等.HPLC测定墨旱莲配方颗粒中的原儿茶酸和原儿茶醛[J].华西药学杂志,2013,28(5):514-516.
• [13]韩强,习峰敏,张凤,等.HPLC法测定墨旱莲中两个噻吩类化合物的含量[J].沈阳药科大学学报,2015,32(4):285-288.
• [14]袁继承,蒋永和,沈志滨.旱莲草化学成分的研究进展[J].亚太传统医药,2009,5(1):125-128.
• [15]平萍,张廷水,张朝凤,等.蟛蜞菊内酯对四氯化碳致小鼠肝损伤的保护作用[J].中国野生植物资源,2012,31(5):41-43.
• [16]徐汝明,邓克敏,陆阳.墨旱莲活性成分对刀豆蛋白A诱导的小鼠肝损伤的作用[J].上海交通大学学报:医学版,2010,30(1):50-54.