采用UPLC-Q-TOF-MS/MS分析半夏药材中的化学成分  

Chemical Components in Pinelliae Rhizoma by UPLC-Q-TOF-MS/MS

作　　者：翟兴英[1] 张凌[1] 李冰涛[1] 冯育林[1] 徐国良[1] 杨世林[1] 金晨[1] ZHAI Xing-ying;ZHANG Ling;LI Bing-tao;FENG Yu-lin;XU Guo-liang;YANG Shi-lin;JIN Chen(Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China)

机构地区：[1]江西中医药大学,南昌330004

出　　处：《中国实验方剂学杂志》2019年第7期173-183,共11页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家重点基础研究发展计划(973计划)项目(2011CB505302);江西中医药大学重点学科青年教师培养计划项目(2015jzzdxk013);江西中医药大学博士启动基金项目(2015BS007)

摘　　要：目的:采用超高效液相色谱串联四极杆飞行时间高分辨率质谱技术(UPLC-Q-TOF-MS/MS)对半夏的化学成分进行定性分析。方法:采用shim-pack xR-ODSⅢ色谱柱(2. 1 mm×75 mm,1. 6μm),以乙腈-0. 1%甲酸水为流动相进行梯度洗脱,柱温40℃,流速0. 25 m L·min-1,采用电喷雾离子化源,正离子全扫描的一级和二级质谱信息。结果:通过一级精确荷质比和二级的碎片数据、参考文献或数据库,质谱裂解规律和标准品的保留时间,发现90个化学成分,初步定性80个化学成分,分别为7个生物碱类,8个醇醚类,12个脂肪酸甘油脂类,5个黄酮类,12个溶血磷脂酰胆碱类,10个醇氨类,11个氨基酸类,11个酰胺类,其他类型4个化合物。结论:通过UPLC-Q-TOF-MS/MS对半夏化学成分时行分析,发现半夏中含有溶血磷脂酰胆碱类物质,其可引起炎症反应及神经元髓鞘脱失和不同程度变性。可推测其可能与半夏的刺激性毒性相关,同时对半夏化学成分全面分析也为半夏药效物质基础研究和质量控制奠定了一定的基础。Objective:To identify the chemical constituents of Pinelliae Rhizoma(BX)by ultrahighpressure liquid chromatography coupled with electrospray time-of-flight tandem mass spectrometry(UPLC-Q-TOFMS/MS).Method:Chromatograpic separation was performed on a shim-pack xR-ODS Ⅲ column(2.1 mm ×75 mm,1.6 μm)using a gradient elution program with mixtures of acetonitrile and 0.1% formic acid-water as mobile phases at a flow rate of 0.25 mL·min^-1.UPLC-Q-TOF-MS/MS was developed for rapid and highthroughput screening of the preliminary chemical profile of BX in positive ion modes.Result:Ninety chemical components were found in BX,according to the accurate Charge-mass Ratio and the MS/MS data,retention time of reference standard,references or databases,the fragmentation regularities of mass spectra.Eighty were identified preliminarily,including 7 alkaloids,8 poly-alcohols,12 fatty glycerides,5 flavonoids,12 lysophosphatidylcholines(LPCs),10 alcohol amines,11 amino acids,11 amides and 4 other type.Conclusion:LPCs were first found in BX.Because BX has certain toxicity,it is found that BX contains LPCs by analyzing the chemical constituents of BX,which can cause inflammatory reaction and neuronal myelin sheath loss and degeneration.Therefore,the analysis of the chemical composition of BX can explain the causes of the toxicity and provide a foundation for the basic research and quality control of the potency of BX.

关 键 词：超高效液相色谱串联四极杆飞行时间高分辨率质谱技术 半夏 化学成分 毒性 

分 类 号：R284.1[医药卫生—中药学] R289[医药卫生—中医学]