This paper describes the configuration and operation of a combined liquid chromatography/mass spectrometry (LC/MS) system for the identification and isolation of DSP-toxins. In the analytical mode, okadaic acid (OA) and dinophysistoxin-1 (DTX-1) are more selectively and sensitively monitored when compared to LC with fluorescence detection. With less sample preparation, the detection limits are decreased by a factor of 3–5, depending on the matrix. In semipreparative mode, OA and DTX-1 could be isolated from crude extracts of Prorocentrum lima algae using mass-based fraction collection with a purity >98%. Due to this method, reference standards of DSP toxins are now commercially available.
The document details a method using a combined liquid chromatography/mass spectrometry (LC/MS) system to identify and isolate Diarrheic Shellfish Poisoning (DSP) toxins, specifically Okadaic Acid (OA) and Dinophysistoxin-1 (DTX-1). The text explains that this configuration offers more selective and sensitive monitoring compared to LC with fluorescence detection.
The guide covers two operational modes: analytical work for monitoring toxins in shellfish extracts and semipreparative work for isolating pure reference standards from crude algae extracts. It provides specific instrument settings, column details, and mobile phase gradients for both Agilent 1100 HPLC systems used in the setup.
| Column (Analytical) | 150 x 3.0 mm ZORBAX SB-C18, 5 µm |
|---|---|
| Column (Semipreparative) | 50 x 9.4 mm ZORBAX SB-C18, 5 µm |
| Flow rate (Semipreparative) | 7.0 mL/min |
The document focuses on Okadaic Acid (OA) and Dinophysistoxin-1 (DTX-1).
Detection limits are decreased by a factor of 3-5 compared to LC with fluorescence detection.
The isolation method achieves a purity greater than 98%.