冯了性风湿跌打药酒的化学成分鉴定
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篇名: 冯了性风湿跌打药酒的化学成分鉴定
TITLE: Identification of Chemical Constituents in Fengliaoxing Fengshi Dieda Wine
摘要: 目的:鉴定冯了性风湿跌打药酒的化学成分。方法:采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱联用技术(UPLC-Q-Exactive-MS)。色谱柱为ThermoAccucoreaQRP18,流动相为0.1%甲酸水溶液-甲醇(梯度洗脱),流速为0.3mL/min,柱温为30℃,进样量为2μL。离子源为加热电喷雾离子源;离子模式为正、负离子模式;鞘气、辅助气为氮气;正离子模式的喷雾电压为3.5kV,毛细管加热温度为350℃,鞘气压力为35psi,辅气压力为15arb,离子源加热温度为320℃;负离子模式的喷雾电压为3.2kV,毛细管加热温度为350℃,鞘气压力为35psi,辅气压力为15arb,离子源加热温度为300℃。质量轴校准为外标法(质量误差小于5ppm),一级质谱扫描范围为m/z80.0~1200.0(分辨率为70000),二级质谱扫描范围为m/z80.0~1200.0(分辨率为17500),碰撞电压为20、40、60eV。检索中国知网、维普、PubMed等数据库,收集冯了性风湿跌打药酒中各味中药材的化学成分信息,建立化学成分数据库;结合上述成分数据库、相关文献以及对照品的保留时间和质谱裂解规律对化合物结构进行鉴定。结果与结论:从冯了性风湿跌打药酒中共鉴定出59种化合物,包括12种黄酮类(如圣草枸橼苷、橙皮苷)、8种生物碱(如包公藤丙素或凹脉丁公藤碱、麻黄碱、伪麻黄碱)、9种有机酸类(如绿原酸、隐绿原酸、新绿原酸)、7种香豆素类(如花椒毒酚)、4种酯类、4种氨基酸类和15种其他类(如挥发油、萜类、酰胺类等)。UPLC-Q-Exactive-MS技术可快速、准确地鉴别冯了性风湿跌打药酒中的化学成分。
ABSTRACT: OBJECTIVE:To identify t he chemical constituents of Fengliaoxing fengshi dieda wine. METHODS :An ultra-high performance liquid chromatography-quadrupole-electrostatic field orbital trap high-resolution mass spectrometry (UPLC-Q-Exactive- MS)technique was used for identifying chemical constituents of Fengliaoxing fengshi dieda wine. The determination was performed on Thermo Accucore aQ RP 18 column with mobile phase consisted of 0.1% formic acid-methanol (gradient elution )at the flow rate of 0.3 mL/min. The column temperature was 30 ℃,and the sample size was 2 μL. HESI source was adopted,ion mode was positive and negative ion mode ,nitrogen as sheath gas and auxiliary gas. The positive ion mode had spray voltage of 3.5 kV, capillary heating temperature of 350 ℃,sheath gas pressure of 35 psi,auxiliary gas pressure of 15 arb,and ion source heating temperature of 320 ℃. The negative ion mode had spray voltage of 3.2 kV,capillary heating temperature of 350 ℃, sheath gas pressure of 35 psi,auxiliary gas pressure of 15 arb,and ion source heating temperature of 300 ℃. The mass axis was calibrated by external standard method (mass error less than 5 ppm). The scanning range of the first mass spectrometry was m/z 80.0-1 200.0 (the resolution was 70 000),the scanning range of secondary mass spectrometry was m/z 80.0-1 200.0(the resolution was 17 500),and the collision voltage was 20,40,60 eV. Retrieved from CNKI ,VIP,PubMed and other database ,the chemical constituents information of each Chinese traditional medicine in Fengliaoxing fengshi dieda wine were collected to establish chemical constituents database. The structure of the compounds was identified on the basis of above constituents database ,the relevant literature ,retention time of reference substance and MS fragmentation regularity. RESULTS & CONCLUSIONS : Fifty-nine compounds were identified in Fengliaoxing fengshi dieda wine ,including 12 flavones(e.g. neoeriocitrin ,hesperidin.),8 alkaloids (e.g. baogongteng C or erycibellin , ephedrine,pseudoephedrine), 9 organic acids (e.g. chlorogenic acid , cryptochlorogenic acid ,neochlorogenic acid ),7 coumarins(e.g. xanthotoxol), 4 esters, 4 amino acids , and 15 other categories(including volatile oils ,terpenes,amides). UPLC- 5103YX11SF37(17)] Q-Exactive-MS technology can quickly and accurately identify the chemical constituents in Fengliaoxing fengshi dieda wine.
期刊: 2020年第31卷第20期
作者: 刘小妹,杨媛媛,胡静,任慧,崔小敏,陶宏迅,陈志永
AUTHORS: LIU Xiaomei ,YANG Yuanyuan ,HU Jing,REN Hui,CUI Xiaomin ,TAO Hongxun ,CHEN Zhiyong
关键字: 冯了性风湿跌打药酒;超高效液相色谱-四极杆-静电场轨道阱高分辨质谱联用技术;化学成分;鉴定
KEYWORDS: Fengliaoxing fengshi dieda wine ;UPLC-Q-
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