RP-HPLC Determination of Ginkgolic Acid in Ginkgo Biloba L.
摘 要
采用反相高效液相色谱法测定银杏中5种银杏酸的含量。样品用甲醇为提取溶剂回流提取后定容至25 mL,取2 mL用正己烷从含有硅藻土的pH 2~3溶液进行液-液萃取,上清液真空旋干,加甲醇定容至2 mL后,取20 μL进样用Waters Symmetry-C18色谱柱分离,以甲醇-水(88+12,含5%乙酸)为流动相,二极管阵列检测器在波长310 nm处检测。峰面积与5种银杏酸的质量浓度分别在一定范围内呈线性关系,方法的检出限(3S/N)在0.26~1.37 mg·L-1之间。方法的平均回收率为99.2%,测定值的相对标准偏差(n=5)为6.83%。
Abstract
Five ginkgolic acids in ginkgo biloba L. were extracted from the sample with methanol under refluxing. The extract was made up to 25 mL and an aliquot of 2 mL was taken and purified by extraction with n-hexane from a solution containing diatomite at pH 2-3. The supernatant was taken and evaporated to dryness rotationally under vacuum. The residue was dissolved with 2 mL of methanol, and 20 μL of the solution were introduced for RP-HPLC analysis by separation on Waters Symmetry-C18 column with the mobile phase of CH3OH-H2O (88+12, containing φ 5% of HOAc). Contents of the 5 acids were determined by DAD at the wavelength of 310 nm. Linear relationships between values of peak area and mass concentration of 5 ginkgolic acids were kept in the definite range, with detection limit (3S/N) in the range of 0.26-1.37 mg·L-1. The value of average recovery found by standard addition method was 99.2%, with value of RSD (n=5) of 6.83%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 浙江省自然科学基金(Y307602)
收稿日期 2011/6/19
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备注吴晓雯(1986-),女,浙江杭州人,硕士研究生,研究方向为色谱分析。
引用该论文: WU Xiao-wen,SUN Yang,MA Zhen-yi,PAN Zai-fa,WANG Li-li. RP-HPLC Determination of Ginkgolic Acid in Ginkgo Biloba L.[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(8): 932~934
吴晓雯,孙杨,马贞依,潘再法,王丽丽. 反相高效液相色谱法测定银杏中银杏酸[J]. 理化检验-化学分册, 2012, 48(8): 932~934
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参考文献
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【9】仰榴青,吴向阳,陈钧.HPLC法测定白果中银杏酸的含量[J].药物分析杂志, 2004,24(6):636-639.
【10】王志强,黄胜海,张琰.不同工艺提取银杏外种皮中银杏酸及含量的测定[J].现代农业科技, 2009,24:326-328.
【2】仰榴青,吴向阳,陈钧.银杏酸的分光光度法测定[J].分析化学, 2004,32(5):661-664.
【3】李英华,张立国,倪力军.薄层分析法快速分析银杏酸的方法研究[J].华东理工大学学报:自然科学版, 2005,31(3):403-405.
【4】GELLERMAN J L, SCHLENK H. Methods for isolation and determination of anacardic acids[J]. Anal Chem, 1968,40(4):739-743.
【5】仰榴青,吴向阳,陈钧.高效液相色谱法测定银杏外种皮中银杏酸的含量[J].分析化学, 2002,30(8):901-905.
【6】BEEK T A V, WINTERMANS M S. Preparative isolation and dual column high-performance liquid chromatography of ginkgolic acids from ginkgo biloba[J]. Journal of Chromatography A, 2001,930:109-117.
【7】张小利,欧阳臻,杨克迪,等.银杏酸的分离制备及HPLC分析[J].中药材, 2003,26(8):558-559.
【8】HE Jing-ren, XIE Bi-jun. Reversed-phase argentation high-performance liquid chromatography in phytochemical analysis of ginkgolic acids in leaves from ginkgo biloba L.[J]. Journal of Chromatography A, 2002,943:303-309.
【9】仰榴青,吴向阳,陈钧.HPLC法测定白果中银杏酸的含量[J].药物分析杂志, 2004,24(6):636-639.
【10】王志强,黄胜海,张琰.不同工艺提取银杏外种皮中银杏酸及含量的测定[J].现代农业科技, 2009,24:326-328.
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