高等学校化学学报
高等學校化學學報
고등학교화학학보
CHEMICAL JOURNAL OF CHINESE UNIVERSITIES
2014年
4期
730-735
,共6页
方菲菲%杜尚广%戴喜末%郭夏丽%陈焕文%罗丽萍
方菲菲%杜尚廣%戴喜末%郭夏麗%陳煥文%囉麗萍
방비비%두상엄%대희말%곽하려%진환문%라려평
电喷雾萃取电离质谱%莲子%主成分分析%生物碱
電噴霧萃取電離質譜%蓮子%主成分分析%生物堿
전분무췌취전리질보%련자%주성분분석%생물감
Extractive electrospray ionization mass spectrometry%Lotus seed%Principal component analysis%Alkaloid
在无需样品预处理的前提下,直接对莲子醇提液进行电喷雾萃取电离质谱( EESI-MS)检测,并对其中可能存在的生物碱母离子进行串联质谱分析确认,通过主成分分析( PCA)对不同贮藏时间莲子的醇提液进行区分.研究结果表明,电离电压、离子传输管温度和样品进样流速的最佳条件分别为3.5 kV,250℃和5μL/min;串联质谱结果表明莲子醇提液中存在莲心碱、甲基莲心碱、莲心季铵碱、荷叶碱及O-去甲基荷叶碱等生物碱. PCA可将不同贮藏时间的莲子明显区分在二维平面的不同区域.本方法无需样品预处理,可用于复杂基体样品中生物碱的快速鉴定,与化学计量学结合可对不同新陈度的莲子样品进行有效区分.
在無需樣品預處理的前提下,直接對蓮子醇提液進行電噴霧萃取電離質譜( EESI-MS)檢測,併對其中可能存在的生物堿母離子進行串聯質譜分析確認,通過主成分分析( PCA)對不同貯藏時間蓮子的醇提液進行區分.研究結果錶明,電離電壓、離子傳輸管溫度和樣品進樣流速的最佳條件分彆為3.5 kV,250℃和5μL/min;串聯質譜結果錶明蓮子醇提液中存在蓮心堿、甲基蓮心堿、蓮心季銨堿、荷葉堿及O-去甲基荷葉堿等生物堿. PCA可將不同貯藏時間的蓮子明顯區分在二維平麵的不同區域.本方法無需樣品預處理,可用于複雜基體樣品中生物堿的快速鑒定,與化學計量學結閤可對不同新陳度的蓮子樣品進行有效區分.
재무수양품예처리적전제하,직접대련자순제액진행전분무췌취전리질보( EESI-MS)검측,병대기중가능존재적생물감모리자진행천련질보분석학인,통과주성분분석( PCA)대불동저장시간련자적순제액진행구분.연구결과표명,전리전압、리자전수관온도화양품진양류속적최가조건분별위3.5 kV,250℃화5μL/min;천련질보결과표명련자순제액중존재연심감、갑기연심감、연심계안감、하협감급O-거갑기하협감등생물감. PCA가장불동저장시간적련자명현구분재이유평면적불동구역.본방법무수양품예처리,가용우복잡기체양품중생물감적쾌속감정,여화학계량학결합가대불동신진도적련자양품진행유효구분.
To identify alkaloids in lotus seeds rapidly and to distinguish fresh and aged lotus seeds, using self-developed extractive electrospray ionization source, ethanol extracts of lotus seeds were directly analyzed by mass spectrometry without any sample pretreatment. The MS were further analyzed using principal component analysis( PCA) . The results showed that optimum conditions of ionization voltage, capillary temperature and sample flow rate were 3.5 kV, 250 ℃, and 5 μL/min, respectively. Liensinine, neferine, lotusine, nucife-rine and O-demethylation nuciferine were found in the ethanol extracts by tandem mass spectrometry, of which signal intensities showed special change trends. Lotus seeds of different storage time and aging degree were clearly distinguishable from each other by PCA. This method is of high sensitivity and high analytical speed, without complex sample pretreatment. The method in this paper is fast and effective to identify alkaloids in real samples with complicated matrix, and combined with chemometrics, it is also used to distinguish fresh and aged lotus seeds.