摘要
建立了用于质谱分析的尖玻片、毛细管、尖滴管3种基于玻璃尖端电喷雾的离子化新方法。通过模拟实验与实际质谱实验,考察了各种实验条件的影响。在喷雾尖端直径小于0.24 mm时,选择喷雾尖端针与反相电极距离10 mm,喷雾电压4.5 kV,喷雾尖端角度为后部偏上5.0°(尖玻片)~7.5°(细毛细管或尖滴管)、左右角度为0°(均对准中间)。选择奎宁、扁桃酸、安息香、苯丙氨酸等不同类型样品的溶液(正离子检测含1%甲酸,负离子检测含1%氨水)置于玻片上或者毛细管与尖滴管后部容器中,进行尖端喷雾直接分析。样品在正离子与负离子模式下分别得到了相应的质谱信号。尖玻片喷雾适合比较稳定、对空气不敏感的样品;毛细管喷雾和尖滴管喷雾则适合分析粘度较低,甚至不稳定的样品溶液。使用本方法实际分析了盐酸普萘洛尔和盐酸小檗碱片剂的提取溶液。3种玻璃尖端电喷雾方法均不需要载气,结构简单、易于构建、操作方便快速,可方便地用于样品溶液的质谱分析。
Three kinds of glass sharp electrospray ionization devices were built for direct mass spectrometry(MS)analysis using sharp slide,slender capillary and sharp dropper.Through the simulation experiment and mass spectrometry experimental investigation,the influence of the experimental conditions was studied.Under the optimum working conditions such as the electrospray tip diameter was less than 0.24 mm,the distance between the electrospray tip and the MS sample inlet was 10 mm,the electrospray voltage was 4.5 kV,the electrospray capillary angle was about 5.0°-7.5°(upper at back)and the left and right angles were 0°,0.1 mg/mL sample solution(containing 1%formic acid for positive ion detection,or ammonium hydroxide for negative ion detection)could be well analyzed by MS.In positive or negative ion modes,the quinine,mandelic acid,benzoin,phenylalanine and other different types of sample solutions were analyzed by MS.The result showed that quinine,mandelic acid,benzoin,phenylalanine,tartaric acid,2,5-dihydroxybenzoic acid(DHB)and tangeretin could be detected in positive ion mode using sharp dropper electrospray.DHB,phenylalanine,tartaric acid and mandelic acid were detected in negative ion mode.Sharp slide electrospray was suitable for measuring the stable sample in the air,capillary electrospray and sharp dropper electrospray were suitable for detecting many low viscosity sample solution even instable sample.Using the method,the extraction solution of propranolol hydrochloride tablet and berberine hydrochloride tablet was directly analyzed by MS.The results showed that the glass sharp electrospray method had the advantages such as without carrier gas,simple structure,easy to build and operate,rapid analysis,anti-cross pollution,and could be conveniently used for MS analysis.
作者
黄煜宇
肖坤
裴兴丽
韩玉良
龚灿
许旭
HUANG Yu-Yu;XIAO Kun;PEI Xing-Li;HAN Yu-Liang;GONG Can;XU Xu(School of Chemical and Environmental Engineering,Shanghai Institute of Technology,Shanghai 201418,China)
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2018年第4期578-585,共8页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金项目(No.31671928)
上海市自然科学基金项目(No.15ZR1440800)资助~~
关键词
质谱离子化
质谱进样
尖端喷雾
玻璃喷雾
Mass spectrometry ionization
Mass spectrometry injection
Sharp electrospray
Glass electrospray
