高效液相色谱串联质谱法同时测定知柏地黄丸中新芒果苷等9种成分的含量

孙颖光, , 生宁, 支旭然, 苑霖, 杜英峰, 刘敏, 于小涵, 张兰桐*

中国药学杂志 ›› 2014, Vol. 49 ›› Issue (2) : 152-155.

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中国药学杂志 ›› 2014, Vol. 49 ›› Issue (2) : 152-155. DOI: 10.11669/cpj.2014.02.017
论 著

高效液相色谱串联质谱法同时测定知柏地黄丸中新芒果苷等9种成分的含量

  • 孙颖光1, 2, 生宁1, 支旭然1, 苑霖1, 杜英峰1, 刘敏1, 于小涵1, 张兰桐1*
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Simultaneous Determination of Nine Components in Zhibaidihuang Concentrated Pills by HPLC-MS/MS

  • SUN Ying-guang1, 2, SHENG Ning1, ZHI Xu-ran1, YUAN Lin1, DU Ying-feng1, LIU Min1, YU Xiao-han1, ZHANG Lan-tong1*
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摘要

目的 建立高效液相色谱串联质谱法测定知柏地黄浓缩丸中新芒果苷, 芒果苷, 知母皂苷BⅡ, 知母皂苷AⅢ, 小檗碱, 莫诺苷, 马钱苷, 芍药苷和丹皮酚含量的方法。方法 采用Diamonsil C18柱(4.6 mm×150 mm, 5 μm);柱温30 ℃;乙腈-0.1%甲酸水溶液为流动相, 以800 μL·min-1梯度洗脱;质谱条件:采用电喷雾离子源正负离子模式同时进行检测, 多反应监测模式(MRM)用于定量测定。结果 知柏地黄丸中9种成分峰面积与浓度呈良好的线性关系, 在15 min内知柏地黄丸中9种成分峰面积与浓度线性关系良好, r>0.999 3;加样回收率 (n=3)分别为98.33%, 99.73%, 100.1%, 101.2%, 101.2%, 100.2%, 99.90%, 100.6% 和100.5%。RSD值分别为1.99%, 1.57%, 1.21%, 2.73%, 1.76 %, 1.59%, 1.11%, 1.70%和1.05%。结论 该方法简便, 准确, 重现性好, 专属性高, 可用于知柏地黄丸的质量控制。

Abstract

OBJECTIVE To develop a method for the determination of neomangiferin, mangiferin, timosaponin BII, timosaponin AⅢ, berberine, morroniside, loganin, paeoniflorin, and paeonol in Zhibaidihuang concentrated pills(traditional Chinese medicine) by HPLC-MS. METHODS The samples were separated on a Diamonsil C18 column (4.6 mm×150 mm, 5 μm ) by gradient elution using acetonitrile and 0.1% aqueous formic acid as the mobile phase. The column temperature was 30 ℃. The elution program was optimized as follows: 0-2.5 min, linearly changed from A-B(5∶95, V/V) to A-B (55∶45, V/V); 2.5-5 min, linearly changed from A-B (55∶45, V/V) to A-B (95∶5, V/V); and 5-15 min, isocratic elution A-B (95∶5, V/V); then quickly returned to initial A-B (5∶95, V/V). This was followed by an equilibration period of 6 min prior to injection of next sample. The flow rate of mobile phase was set at 0.8 mL·min-1, and the injection volume was 10 μL. Multiple-reaction monitoring (MRM) scanning was employed for quantification with switching electrospray ion source polarity between positive and negative modes in a single run. RESULTS There was significant correlation between the peak area and concentration of each compound within the test range (r>0.999 3). The average recoveries (n=3) of the nine compounds were 98.33%, 99.73%, 100.1%, 101.2 %, 101.2%, 100.2%, 99.90%, 100.6% and 100.5%, respectively. The RSDs were 1.99%, 1.57%, 1.21%, 2.73%, 1.76%, 1.59%, 1.11%, 1.70% and 1.05%, respectively. CONCLUSION The method is simple, accurate and highly reproducible, and can be used for the determination of nine compounds in Zhibaidihuang concentrated pills.

关键词

液质联用 / 知柏地黄丸 / 含量测定 / 新芒果苷 / 芒果苷

Key words

HPLC-MS/MS / Zhibaidihuang concentrated pill / determination / neomangiferiu / mangiferin

引用本文

导出引用
孙颖光, , 生宁, 支旭然, 苑霖, 杜英峰, 刘敏, 于小涵, 张兰桐*. 高效液相色谱串联质谱法同时测定知柏地黄丸中新芒果苷等9种成分的含量[J]. 中国药学杂志, 2014, 49(2): 152-155 https://doi.org/10.11669/cpj.2014.02.017
SUN Ying-guang, , SHENG Ning, ZHI Xu-ran, YUAN Lin, DU Ying-feng, LIU Min, YU Xiao-han, ZHANG Lan-tong*. Simultaneous Determination of Nine Components in Zhibaidihuang Concentrated Pills by HPLC-MS/MS[J]. Chinese Pharmaceutical Journal, 2014, 49(2): 152-155 https://doi.org/10.11669/cpj.2014.02.017
中图分类号: R917   

参考文献

Ch.P(2010) VolⅠ(中国药典2010年版. 一部) . 2010: 820. LI M Q. Research of Zhibaidihuang concentrated pill . Tradit Chin Med Res (中医研究), 1997, 10(5):56-57. CHEN Y R, LIU H Q. Detection of mangiferin in Zhibaidihuang Pill by RP-HPLC . Chin J Hosp Pharm(中国医院药学杂志), 2008, 28(8):677-679. CHEN X Y. Content determination of sarsasapogenin in Zhibai Dihuang Pills by HPLC . J China Pharm (中国药房), 2011, 22(40):3826-3827. LIU Y M. Assay of paeonol in Zhibai Dihuang Pills by thin layer scanning chromatography .Hebei J Tradit Chin Med(湖北中医杂志), 2005, 27(7):52-54. XU G X, YANG J, CHEN Z W. Determining the contents of loganin in Zhibodihuang Concentrated Pill by HPLC . J Henan Univ Chin Med (河南中医学院学报), 2007, 22(4):30. HONG J. Determining the contents of paeonol in Zhibaidihuang concentrated pill by HPLC . Strait Pharm J (海峡药学), 2008, 20(8):31-33. CHEN Q H, TANG Y J. HPLC Determination of berberine hydrochloride and palmatine hydrochloride in Zhibai Dihuang pills . Chin J Pharm Anal (药物分析杂志), 2012, 32(12):2198-2202. WENG X M, LI Z L. Determination of content of berberine hydrochloride and paeonol in Zhibai Dihuang Wan by HPLC . Chin J Hosp Pharm (中国医院药学杂志), 2001, 21(1):21-22. SUN Y G, DU Y F, LIU Y, et al. Simultaneous determination of 9 components in Anemarrhena asphodeloides by liquid chromatography-tandem mass spectrometry combined with chemometric techniques. J Sep Sci, 2012, 35:1796-1807. YI B, SUN H, YUAN Y, et al. Determination of neomangiferin, mangiferin and berberine hydrochloride in traditional medicine partner of Rhizoma Anemarrhenal and Cortex Phellodendri using RP-HPLC . Chin Tradit Herb Drugs (中草药), 2007, 38(6):856-858. LAO F Y, LI X N, ZHANG W G, et al. Determination of content of morroniside and loganin in total glucosides from Cornus officinalis by HPLC . Chin J Public Health(中国公共卫生), 2009, 25(7):889-891. YANG Z S, PENG Z H, YAO Q H, et al. Research progress of pharmacological effects of paeonol . Chin Rem Clin (中国药物与临床), 2011, 11(5):545-554.

基金

河北省自然科学基金-石药集团医药联合研究基金(H2012206079)
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