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Improved conditions for the application of solid phase microextraction prior to HPLC–FLD analysis of anatoxin-a

✍ Scribed by Sandra Rellán; Ana Gago-Martínez

Publisher
John Wiley and Sons
Year
2007
Tongue
English
Weight
770 KB
Volume
30
Category
Article
ISSN
1615-9306

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✦ Synopsis

Abstract

Solid phase microextraction coupled with high performance liquid chromatography with fluorescence detection has been optimized and evaluated for a simple, rapid, and selective analysis of anatoxin‐a. Four kinds of fiber (100 μm polydimethylsiloxane, 60 μm polydimethylsiloxane/divinylbenzene, 50 μm Carbowax/templated resin‐100, and 85 μm polyacrylate) were evaluated for an efficient extraction of the toxin. Parameters relating to the desorption step, such as desorption mode, solvent composition, time for both static and dynamic desorption, as well as carryover, have been studied and optimized. The derivatization process was investigated using NBD‐F as derivatizing reagent. Anatoxin‐a derivative was formed when the anatoxin‐a‐loaded fiber was inserted in a vial containing 5 μL of NBD‐F. Variables affecting extraction such us ionic strength, temperature, and time have been also optimized. The results obtained showed linearity in the range of 10–2000 ng and a limit of detection of 0.29 ng/mL in river water. The presented method has been applied to different environmental samples.

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## Abstract Solid‐phase microextraction (SPME) has been directly coupled to an ion‐trap mass spectrometer (MS) for the determination of the model compound lidocaine in urine, hereby applying MS/MS [fragmentation of [M + H]^+^ (__m/z__ 235) to a fragment with __m/z__ 86]. The throughput of samples h