Micro-SPE Method for Sample Introduction in Capillary HPLC/MS

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• 作者：Achille Cappiello ; Arnaldo Berloni ; Giorgio Famiglini ; Filippo Mangani ; and Pierangela Palma
• 刊名：Analytical Chemistry
• 出版年：2001
• 出版时间：January 15, 2001
• 年：2001
• 卷：73
• 期：2
• 页码：298 - 302
• 全文大小：60K
• 年卷期：v.73,no.2(January 15, 2001)
• ISSN：1520-6882

文摘

A new solid-phase extraction on-line device for micro-HPLC is presented. This device optimizes the injectionof very dilute samples into a packed capillary column. Itconsists of two capillary, reversed-phase, HPLC columnsof different length that can be linked together as a singlechromatographic column. The first segment, only 2 cmlong is connected to the HPLC injector. When disconnected from the longer column, several milliliters of anaqueous sample can be passed through at a high flow ratefor fast trapping. On the basis of the retention mechanism,all suitable compounds are focused on the short columnhead in a sharp band. As soon as the chromatographiccolumn is recomposed, the trapped analytes are elutedand separated at the optimal flow rate and gradientconditions. Due to the high preconcentration factor, trace-level analysis can be performed successfully. Differentclasses of analytes of various polarities and molecularweights can be determined, depending on the stationaryphase and on the detector used. Some pesticides belonging to different classes were chosen to evaluate theperformance of the device using an electron ionizationmass spectrometer as HPLC detector. A fungicide in anirrigation canal water was determined at a concentrationlevel of 4.5 g·L^-1.