摘要
目的:对11-乙氧基缬草醛、11-甲氧基缬草醛、去酰基缬草醛和缬草醛在电喷雾质谱下的裂解途径进行探讨。方法:采用超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(UHPLC-LTQ Orbitrap MS)对4个缬草醛类对照品进行系统研究。色谱条件:采用UPLC BEH-C_(18)色谱柱(1.7μm,2.1 mm×100 mm),流动相A为0.1%甲酸水溶液,B为乙腈,洗脱条件(0~20 min,85%A→50%A;20~25 min,50%A→20%A,25~30 min,20%A),流速为0.3 m L·min^(-1),柱温30℃,检测波长288 nm,进样量2μL。结果:4个缬草醛类成分在正离子模式下均会形成m/z 177、149、78等基本碎片离子,而11-乙氧基缬草醛和11-甲氧基缬草醛主要形成m/z 161、m/z 133、m/z 105特征碎片离子,而去酰基缬草醛和缬草醛则会形成m/z 131、m/z 103等特征碎片离子。结论:该类化合物有着较强的裂解规律,可用于缬草醛类化合物的快速结构鉴定。
Objective：To explore the fragmentation pathways of 11-ethoxyviburtinal,11-methoxyviburtinal,desacylbaldrinal and baldrinal by electrospray ionization mass spectrometry.Methods：Four reference standards were systematically investigated by ultra high performance liquid chromatography combined with linear ion trap electrostatic field orbit trap high resolution mass spectrometry（UHPLC-LTQ Orbitrap MS）.UPLC analysis was performed on a BEH-C_（18） column（1.7 μm,2.1 mm×100 mm）,with a mobile phase consisting of 0.1% formic acid（A）-acetonitrile（B） at the flow rate of 0.3 m L·min-（-1）（0-20 min,85%A → 50%A;20-25 min,50%A → 20%A;25-30 min,20%A）.The detection wavelength was 288 nm and the column temperature was controlled at 30 ℃,and the injection volume was 2 μL.Results：The fragment ions of m/z 177,m/z 149 and m/z 78 were found in four baldrinals in positive ion mode,while the fragment ions m/z 161,m/z 133 and m/z 105 were found in 11-ethoxyviburtinal and 11-methoxyviburtinal and m/z 131 and m/z 103 were found in desacylbaldrinal and baldrinal.Conclusion：This kind of compound has strong fragmentation regularity,which can be used for the rapid structure identification of baldrinals.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第2期234-240,共7页
Chinese Journal of Pharmaceutical Analysis
基金
国家自然科学基金资助项目(No.81374044)
北京中医药大学自主选题项目(2016-JYB-JSMS-013)
关键词
蜘蛛香
缬草醛
乙氧基缬草醛
甲氧基缬草醛
去酰基缬草醛
结构鉴定
LTQ-Orbitrap质谱
电喷雾多级质谱
裂解途径
Valerianae Jatamansi Rhizoma et Radix
baldrinal
ethoxyviburtinal
methoxyviburtinal
desacylbaldrinal
structure identification
LTQ-orbitrap mass spectrometry
electrospray ionization tandem massspectrometry
fragmentation pathway
