UPLC-QTRAP-MS/MS法同时测定苍耳类药材中酚酸、蒽醌及黄酮类成分

刘娟秀, 罗益远, 刘训红, 宋建平, 华愉教, 王胜男

刘娟秀, 罗益远, 刘训红, 宋建平, 华愉教, 王胜男. UPLC-QTRAP-MS/MS法同时测定苍耳类药材中酚酸、蒽醌及黄酮类成分[J]. 质谱学报, 2016, 37(6): 542-553. DOI: 10.7538/zpxb.youxian.2016.0026
引用本文: 刘娟秀, 罗益远, 刘训红, 宋建平, 华愉教, 王胜男. UPLC-QTRAP-MS/MS法同时测定苍耳类药材中酚酸、蒽醌及黄酮类成分[J]. 质谱学报, 2016, 37(6): 542-553. DOI: 10.7538/zpxb.youxian.2016.0026
LIU Juan-xiu, LUO Yi-yuan, LIU Xun-hong, SONG Jian-ping, HUA Yu-jiao, WANG Sheng-nan. Simultaneous Determination of Phenolic Acids, Anthraquinones and Flavonoids in Xanthii Herba and Xanthii Fructus by UPLC-QTRAP-MS/MS[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 542-553. DOI: 10.7538/zpxb.youxian.2016.0026
Citation: LIU Juan-xiu, LUO Yi-yuan, LIU Xun-hong, SONG Jian-ping, HUA Yu-jiao, WANG Sheng-nan. Simultaneous Determination of Phenolic Acids, Anthraquinones and Flavonoids in Xanthii Herba and Xanthii Fructus by UPLC-QTRAP-MS/MS[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 542-553. DOI: 10.7538/zpxb.youxian.2016.0026
刘娟秀, 罗益远, 刘训红, 宋建平, 华愉教, 王胜男. UPLC-QTRAP-MS/MS法同时测定苍耳类药材中酚酸、蒽醌及黄酮类成分[J]. 质谱学报, 2016, 37(6): 542-553. CSTR: 32365.14.zpxb.youxian.2016.0026
引用本文: 刘娟秀, 罗益远, 刘训红, 宋建平, 华愉教, 王胜男. UPLC-QTRAP-MS/MS法同时测定苍耳类药材中酚酸、蒽醌及黄酮类成分[J]. 质谱学报, 2016, 37(6): 542-553. CSTR: 32365.14.zpxb.youxian.2016.0026
LIU Juan-xiu, LUO Yi-yuan, LIU Xun-hong, SONG Jian-ping, HUA Yu-jiao, WANG Sheng-nan. Simultaneous Determination of Phenolic Acids, Anthraquinones and Flavonoids in Xanthii Herba and Xanthii Fructus by UPLC-QTRAP-MS/MS[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 542-553. CSTR: 32365.14.zpxb.youxian.2016.0026
Citation: LIU Juan-xiu, LUO Yi-yuan, LIU Xun-hong, SONG Jian-ping, HUA Yu-jiao, WANG Sheng-nan. Simultaneous Determination of Phenolic Acids, Anthraquinones and Flavonoids in Xanthii Herba and Xanthii Fructus by UPLC-QTRAP-MS/MS[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 542-553. CSTR: 32365.14.zpxb.youxian.2016.0026

UPLC-QTRAP-MS/MS法同时测定苍耳类药材中酚酸、蒽醌及黄酮类成分

Simultaneous Determination of Phenolic Acids, Anthraquinones and Flavonoids in Xanthii Herba and Xanthii Fructus by UPLC-QTRAP-MS/MS

  • 摘要: 建立了超高效液相色谱-三重四极杆-线性离子阱质谱(UPLC-QTRAP-MS/MS)同时测定苍耳草、苍耳子药材中酚酸、蒽醌及黄酮类18种活性成分的方法。采用Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm×5 μm),以甲醇0.2%甲酸水溶液为流动相,梯度洗脱,柱温为35 ℃,选择电喷雾离子源(ESI),负离子多反应监测(MRM)扫描方式检测。结果表明:在一定的浓度范围内,18种目标化合物的线性关系良好,线性相关系数均大于0.999 4,精密度、重复性和稳定性的RSD值均小于3%;加样回收率在96.81%~102.78%之间,RSD小于3%。该方法简便准确、灵敏度高、重复性好,适用于苍耳类药材中多元活性成分的同时测定,可为苍耳类药材内在质量的综合评价和全面控制提供方法参考。
    Abstract: A comprehensive analytical method based on UPLC-QTRAP-MS/MS was developed for the simultaneous determination of eighteen bioactive components including phenolic acids, anthraquinones and flavonoids in Xanthii Herba and Xanthii Fructus. Under the optimized chromatographic conditions, extracts of eighteen target components were obtained on an Agilent ZORBAX SB-C18 column (250 mm×4.6 mm×5 μm) using methanol-0.2% formic acid as mobile phases for gradient elution. The flow rate was 1.0 mL/min and the column temperature was 35 ℃. The target compounds were analyzed in the negative ion multiple reaction monitoring (MRM) mode. The results show that eighteen components have good linearity, the correlation coefficients of all the calibration curves are higher than 0.999 4. Relative standard deviations (RSDs) of precision, repeatability and stability are lower than 3%. The recoveries range from 96.81% to 102.78%, and the RSDs are less than 3%. The established method is accurate, sensitive, and has good repeatability. It is suitable for simultaneous determination of eighteen components in Xanthii Herba and Xanthii Fructus, which can provide a reliable and effective technique for the quality control of Xanthii Herba and Xanthii Fructus.
  • [1] 国家药典委员会. 中华人民共和国药典2015版(一部)[M]. 北京:中国医药科技出版社,2015:162.
    [2] 南京中医药大学. 中药大辞典[M]. 上海:上海科学技术出版社,2005:1486-1488.
    [3] 苏新国,宓穗卿,王宁生,等. 苍耳子药用研究进展[J]. 中药新药与临床药理,2006,17(1):68-72.SU Xinguo, MI Suiqing, WANG Ningsheng, et al. Review on the pharmaceutical study development of Frucutus Xanthii[J]. Traditional Chinese Drug Research & Clinical Pharmacology, 2006,17(1): 68-72(in Chinese).
    [4] 阮贵华,李攻科. 苍耳子的化学成分及其分离分析研究进展[J]. 中成药,2008,30(3):421-426.RUAN Guihua, LI Gongke. Advances in studies on chemical composition, segregation and analysis research of Frucutus Xanthii[J]. Chinese Traditional Patent Medicine, 2008, 30(3): 421-426(in Chinese).
    [5] 杨柳,吴金雄,许舜军,等. 苍耳子中酚酸类化合物的鉴别及绿原酸的含量测定[J]. 中国实验方剂学杂志,2011,17(19):85-88.YANG Liu, WU Jinxiong, XU Shunjun, et al. Characterization of phenolic acids and quantitative analysis of chlorogenic acid contained in Frucutus Xanthii[J]. Chinese Journal of Experimental Traditional Medical Formulae, 2011, 17(19): 85-88(in Chinese).
    [6] 黄文华,余竞光,孙兰,等. 中药苍耳子化学成分的研究[J]. 中国中药杂志,2005,30(13):1027-1028.HUANG Wenhua, YU Jingguang, SUN Lan, et al. Study the chemical composition of traditional Chinese medicine Frucutus Xanthii[J]. China Journal of Chinese Materia Medica, 2005, 30(13): 1027-1028(in Chinese).
    [7] 韩婷,李慧梁,胡园,等. 苍耳子中酚酸类化合物及不同品种和居群苍耳子中总酚酸含量的测定[J]. 中国中西医结合学报,2006,4(2):194-198.HAN Ting, LI Huiliang, HU Yuan, et al. Phenolic acids in Frucutus Xanthii and determination of contents of total phenolic acids in diffenert species and populations of Xanthium in China[J]. Journal of Chinese Integrative Medicine, 2006, 4(2): 194-198(in Chinese).
    [8] 宋琳琳,沙靖全,赵宏,等. 苍耳草中总酚酸的含量测定及其抗炎作用研究[J]. 时珍国医国药,2013,24(10):2331-2332.SONG Linlin, SHA Jingquan, ZHAO Hong, et al. Determination of TPA content of Xanthium sibiricum Patrin exWidder and anti-inflammatory effect[J]. Lishizhen Medicine and Materia Medica Research, 2013, 24(10): 2331-2332(in Chinese).
    [9] 曹亮,周建军. 蒽醌类化合物的研究进展[J]. 西北药学杂志,2009,24(3):237-238.CAO Liang, ZHOU Jianjun. Progress anthraquinone compounds[J]. Northwest Pharmaceutical Journal, 2009, 24(3): 237-238(in Chinese).
    [10] 钟地长,张淑凤,陈振锋,等. 天然产物黄酮类化合物的提取、纯化及其金属配合物的研究进展[J]. 化学世界,2006,47(9):56-59.ZHONG Dichang, ZHANG Shufeng, CHEN Zhenfeng, et al. Research progress on the extraction and purification of natural flavonoides and their metal complexes[J]. Chemical World, 2006, 47(9): 56-59(in Chinese).
    [11] 王如阳,刘晓芳,刘满红,等. 苍耳子提取液的抗氧化活性研究与总黄酮含量测定[J]. 云南中医中药杂志,2008,29(9):42-43.WANG Ruyang, LIU Xiaofang, LIU Manhong, et al. Study on the antioxidant activity of the extract and determine the content of total flavonoids of Fructus Xanthii[J]. Yunnan Journal of Traditional Chinese Medicine and Materia Medica, 2008, 29(9): 42-43(in Chinese).
    [12] 仝俊太,徐圣秋,李伟东,等. 高效液相色谱法测定苍耳草中绿原酸的含量[J]. 中国医院药学杂志,2011,31(20):1739-1740.TONG Juntai, XU Shengqiu, LI Weidong, et al. Determination of chlorogenic acid in Xanthium herba by HPLC[J]. Chinese Journal of Hospital Pharmacy, 2011, 31(20): 1739-1740(in Chinese).
    [13] 明乾良,高翔,张宏,等. 用HPLC法测定不同地区三种苍耳子中绿原酸的含量[J]. 药学服务与研究,2008,8(4):258-260.MING Qianliang, GAO Xiang, ZHANG Hong, et al. Determination of chlorogenic acid in three species of cocklebur fruits from different regions of China by HPLC method[J]. Pharmaceutical Care and Research, 2008, 8(4): 258-260(in Chinese).
    [14] 王虹,何桂霞,姚颖. 苍耳子中总蒽醌的含量测定[J]. 中国现代药物应用,2009,3(1):89-90.WANG Hong, HE Guixia, YAO Ying. Determination of total anthraquinones in Xanthii Fructus[J]. Chinese Journal of Modern Drug Application, 2009, 3(1): 89-90(in Chinese).
    [15] 尹靖先,邓晓鸿,车晓彦,等. 苍耳子的薄层层析鉴别研究[J]. 华西药学杂志,2005,20(1):67-69.YIN Jingxian, DENG Xiaohong, CHE Xiaoyan, et al. Study on TLC identification of Fructus Xanthii[J]. West China Journal of Pharmaceutical Sciences, 2005, 20(1): 67-69(in Chinese).
    [16] 李贵花,郑轩. 响应面法优化苍耳子总黄酮超声辅助提取工艺[J]. 西北民族大学学报:自然科学版,2015,36(97):53-58.LI Guihua, ZHENG Xuan. Optimization of ultrasonic assisted extraction of flavonoids from Fructus Xanthii by response surface methodoly[J]. Journal of Northwest University for Nationalities: Natural Science, 2015, 36(97): 53-58(in Chinese).
    [17] 张成,朱科谕,张庞文,等. 苍耳子、田基黄中黄酮类物质提取含量测定及对比研究[J]. 中国农学通报,2014,30(6):306-313.ZHANG Cheng, ZHU Keyu, ZHANG Pangwen,et al. The study on determination content of flavonoids extracts from Fructus Xanthii and Hypericum japonicum Thumb[J]. Chinese Agricultural Science Bulletin, 2014, 30(6): 306-313(in Chinese).
    [18] 田静,夏玉凤,房克慧. HPLC法同时测定苍耳类药材中8种酚酸类成分的含量[J]. 中药材,2013,36(10):1623-1626.TIAN Jing, XIA Yufeng, FANG Kehui. Simultaneous determineation of 8 phenolic acids in Xanthium sibiricum medicines by HPLC[J]. Jorunal of Chinese Medicinal Materials, 2013, 36(10): 1 623-1 626(in Chinese).
    [19] 朵睿,刘玉红,王明奎,等. HPLC 同时测定苍耳子中6个化学成分的含量[J]. 药物分析杂志,2013,33(1):78-82.DUO Rui, LIU Yuhong, WANG Mingkui, et al. HPLC simultaneous determination of the content of 6 constituents in Fructus Xanthii[J]. Chinese Journal of Pharmaceutical Analysis, 2013, 33(1): 78-82(in Chinese).
    [20] 杨柳,苏芝军,许舜军,等. UPLC法同时测定苍耳子中4 种酚酸类成分的含量[J]. 药学学报,2010,45(12):1537-1540.YANG Liu, SU Zhijun, XU Shunjun, et al. Simultaneous determination of 4 phenolic acids in Cangerzi by ultra-performance liquid chromatography[J]. Acta Pharmaceutica Sinica, 2010, 45(12): 1537-1540(in Chinese).
    [21] 秦泗涟,马利华,王振中,等. UPLC 法同时测定炒苍耳子配方颗粒中5种酚酸类成分[J]. 中成药,2012,34(7):1393-1395.QIN Silian, MA Lihua, WANG Zhenzhong, et al. UPLC Determination fried cocklebur Granule 5 kinds of phenolic acids[J]. Chinese Traditional Patent Medicine, 2012, 34(7): 1393-1395 (in Chinese).
    [22] 洪燕,韩燕全,夏伦祝,等. 超高效液相色谱法同时测定不同产地苍耳子9种酚酸类成分的含量[J]. 中国药学杂志,2013,48(13):1109-1112.HONG Yan, HAN Yanquan, XIA Lunzhu, et al. Simultaneous determination of nine phenolic acid components in Xanthii Fructus[J]. Chinese Pharmaceutical Journal, 2013, 48(13): 1109-1112(in Chinese).
    [23] 刘娟秀,罗益远,刘训红,等. 毛细管电泳同时测定苍耳类药材中7种酚酸类成分的含量[J]. 中国药学杂志,2015,50(4):366-370.LIU Juanxiu, LUO Yiyuan, LIU Xunhong, et al. Simultaneous determination of seven phenolic acids from Xanthii Herba and Xanthii Fructus by HPCE[J]. Chinese Pharmaceutical Journal, 2015, 50(4): 366-370(in Chinese).
    [24] 项赟,李立军,再帕尔•阿不力孜. 液相色谱-质谱联用方法在药用植物成分分析中的作用[J]. 药学学报,2002,37(5):389-395.XIANG Yun, LI Lijun, ZEPER Abliz. Application of LC-MS in the analysis of constituents of crude plant extracts[J]. Acta Pharmaceutica Sinica, 2002, 37(5): 389-395(in Chinese).
    [25] 苏建,袁志芳,张兰桐,等. RP-HPLC法测定何首乌和夜交藤中二苯乙烯苷和蒽醌类成分[J]. 中草药,2007,38(2):278-281.SU Jian, YUAN Zhifang, ZHANG Lantong, et al. Determination of stilbeneglycoside and anthraquinone in Polygonum multiflorum Thunb by RP-HPLC[J]. Chinese Tradit Herbal Drugs, 2007, 38(2): 278-281(in Chinese).
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  • 刊出日期:  2016-11-19

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