目的 建立胶束电动毛细管色谱二极管阵列检测法(MEKC-DAD)同时测定女贞子饮片中红景天苷、酪醇、女贞苷、特女贞苷、齐墩果酸和熊果酸含量的方法。方法 60 mmol·L-1硼砂-10 mmol·L-1十二烷基硫酸钠(SDS)-30 mmol·L-1羟丙基-β-环糊精-10%的甲醇(pH 9.03)为电泳介质, 未涂渍标准熔融石英毛细管(75 μm×64.5 cm, 有效长度56 cm)为分离通道, 分离电压为20 kV, 检测波长为210 nm, 毛细管温度为25 ℃, 压力进样为5 kPa×6 s。结果 6种指标成分的浓度与峰面积的线性关系良好(r＞0.95);加样回收率为94.57%～102.07% (RSD<5%);用此法测定了女贞子饮片中6种指标成分的含量, 结果满意。结论 该方法准确、可靠, 重复性较好, 可用于女贞子饮片内在质量的评价和控制。
Abstract
OBJECTIVE To establish a micellar electrokinetic chromatography(MEKC) method for simultaneous determination of salidroside, tyrosol, ligustroflavone, specnuezhenide, oleanolic acid, and ursolic acid in Ligustri Lucidi Fructus. METHODS 60 mmol·L-1 borax-10 mmol·L-1 SDS-30 mmol·L-1 hydroxypropyl-beta-cyclodextrin-10% methyl alcohol was used as the buffer solution (pH 9.03). Uncoated fused silica capillary (75 μm×64.5 cm, 56 cm of effective length) was used with separation voltage of 20 kV. The detection wavelength was set at 210 nm. The column temperature was maintained at 25 ℃, and the sample was injected at 5 kPa×6 s. RESULTS The calibration curves of the six index components showed good linearity (r＞0.95) in the range of the tested concentrations, and the average recoveries of the method were between 94.57% and 102.07% (RSD<5%). CONCLUSION The method is simple, accurate and reproducible, and can be used for the quality control of Ligustri Lucidi Fructus.
关键词
胶束毛细管电泳法 /
女贞子 /
指标成分 /
含量测定 /
红景天苷 /
酪醇 /
女贞苷 /
特女贞苷 /
齐墩果酸 /
熊果酸
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Key words
high performance capillary electrophoresis(HPCE) /
Ligustri Lucidi Fructus /
index component /
content determination /
salidroside /
tyrosal /
ligustroflavone /
specnuezhenide /
oleanolic acid /
ursolic acid
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中图分类号：
R917
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参考文献
[1] DAI C F, YANG X Y. The recent research developments in Ligustrum lucidum Ait. Shanxi J Tradit Chin Med(山西中医药学报), 1999, 2(15): 13-14.[2] YING S, TANG X Z, WU L J. Chemical constituents from Ligustrum lucidum Ait. J Shenyang Pharm Univ(沈阳药科大学学报), 1995, 12(2): 125-126.[3] LIU J, LIU Y, PARKINSON A, et al. Effect of oleanolic acid on hepatic toxicant-activating and detoxifying systems in mice. J Pharmacol Exp Ther, 1995, 275 (2):768-774.[4] JIN Z G, JIN J, XIAO Z G, et al.Advances in research on pharmacological effects and clinical application of Ligustri Lucidi Fructus. Pharm Care Res(药学服务与研究), 2011, 11(3):189-191.[5] XU W C, CHU Y J, LIN D, et al. Study on separation performance of capillary column coated physically with modified hyperbranched polycarbosilane. Chin J Anal Chem(分析化学), 2010, 38(8): 1167-1169.[6] HUANG W, SU Z R, BI W C, et al. HPLC Determination of nuezhenide in Fructus Ligustri Lucidi. Chin J Pham Anal(药物分析杂志), 2009, 29(5): 35-37.[7] HUANG B M, YAO C W, BIAN Q Q, et al. Determination of oleanolic acid in Ligustrum lucidum by capillary electrophoresis with amperometric detection. Chem Res Appl(化学研究与应用), 2011, 3(23):1156-1157.[8] LIU W, CUI Y X, CHEN Z H, et al. HPCE for the content determination of oleanolic acid, ursolic acid and rosmarinic acid in spica prunellae from different origins. J Chin Med(中医学报), 2011, 26(12): 135-136.[9] QI Z H, WANG S W. Determination of oleanolic acid and ursolic acid in the fruits of Ligustrum lucidum Ait. of Shanxi by HPLC. Chin J Info Tradit Chin Med(中国中医药信息杂志), 2007, 14(5):516-518.
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脚注
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基金
江苏省中药炮制重点实验室开放式课题(ZYPZ007);江苏省科技厅“科技基础实施建设计划”专项(BM2009903);江苏高校优势学科建设工程资助项目(ysxk-2010)
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