狗脊毛甲醇提取物UPLC/Q-TOF-MS分析  

Analysis of Chemical Composition in Methanol Extract of Yellow Hairs from Rhizome of Cibotii Rhizoma by UPLC/Q-TOF-MS

作　　者：徐钢[1] 孙娜[1] 赵敏杰[1] 林桂梅[1] 高慧[1] 贾天柱[1] 

机构地区：[1]辽宁中医药大学药学院,国家中医药管理局中药炮制重点研究室,辽宁省中药炮制工程技术研究中心,辽宁大连116600

出　　处：《中国实验方剂学杂志》2014年第7期46-50,共5页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家自然科学基金项目(30973938)

摘　　要：目的：探索狗脊毛化学成分组成及其外用止血的物质基础。方法：采用超声、索氏、回流3种方式对狗脊毛进行甲醇提取，通过UPLC/Q-TOF-MS对各提取物进行定性分析，流动相乙腈（A）-水（B）梯度洗脱（0-5 min，5%-55% A；5-7 min，55%-85% A；7-15 min，85%-100% A；15-20 min，100% A），检测波长254 nm，m/z扫描范围100-1 000，脱溶剂气温度350 ℃，脱溶剂气体积流量9 L·min^-1，喷雾器压力2.4×10^5Pa，毛细管电压4 000 V。结果：3种方式共检出化合物50个，给出了其中38个化合物的推荐分子式和名称。编号32~39共8个化合物为一系列三酰基甘油类同系物。结论：狗脊毛中化合物包括植物油类（三酰基甘油）、有机酸类、有机酸酯类、生物碱类、黄酮类、多酚类、糖苷类等，相对分子质量集中于200-800，三酰基甘油可能为主要药效成分。Objective： To explore chemical composition in yellow hairs of rhizome of Cibotii Rhizoma and its material basis for topical hemostatic effect. Method： Chemical composition in yellow hairs of rhizome of Cibotii Rhizoma was extracted by ultrasound,Soxhlet＇s extractor and reflux methanol extraction technologies,each extract was determined by UPLC/Q-TOF-MS for qualitative analysis,mobile phase of acetonitrile（A）-water（B） gradient elution（0-5 min,5%-55% A;5-7 min,55%-85% A;7-15 min,85%-100% A;15-20 min,100% A）,detection wavelength was 254 nm,scanning range of m/z from 100 to 1 000,desolvation gas temperature at 350 ℃,volume flow of desolvation gas was 9 L·min^-1,spray pressure was 2.4×10^5 Pa,capillary voltage was 4 000 V. Result： A total of 50 compounds were checked out by these three methods,38 compounds out of them were recommended for molecular formula and name.Eight compounds of Number 32-39 should be a series of triacylglycerols homologues. Conclusion： Relative molecular weight was concentrated within 200-800,including vegetable oils（triacylglycerols）,organic acids,organic acid esters,alkaloids,flavonoids,polyphenols,glycosides and so on,triacylglycerols of which may be the main ingredient in yellow hairs of rhizome of Cibotii Rhizoma.

关 键 词：狗脊毛 甲醇提取物 三酰基甘油 超高效液相-四级杆-飞行时间串联质谱 定性分析 

分 类 号：R284.1[医药卫生—中药学]