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通过液相色谱-电喷雾质谱联用及紫外检测法,对从海水和双鞭毛藻(强壮鳍藻)中固相萃取后的pectenotoxin-2进行测定。扇贝中pectenotoxin-2氧化为pectenotoxin-6的证据。

Determination of pectenotoxin-2 after solid-phase extraction from seawater and from the dinoflagellate Dinophysis fortii by liquid chromatography with electrospray mass spectrometry and ultraviolet detection. Evidence of oxidation of pectenotoxin-2 to pectenotoxin-6 in scallops.

作者信息

Suzuki T, Mitsuya T, Matsubara H, Yamasaki M

机构信息

Tohoku National Fisheries Research Institute, Miyagi, Japan.

出版信息

J Chromatogr A. 1998 Jul 31;815(1):155-60. doi: 10.1016/s0021-9673(98)00010-7.

Abstract

Solid-phase extraction of pectenotoxin-2 (PTX2) and pectenotoxin-6 (PTX6) from seawater samples using a nonpolar cartridge column Sep-Pak C18 was investigated for determination of PTXs in toxic phytoplankton. PTX2 and PTX6 were almost completely recovered from the seawater samples. Determinations of PTX2 from the toxic phytoplankton and scallops were carried out by liquid chromatography (LC) on UV trace equipped with an atmospheric pressure electrospray ionization mass spectrometry (ESI-MS). PTX2 obtained from the toxic phytoplankton and scallops yielded a mass spectra exhibiting abundant [M+H]+, [M+NH4]+ and [M+Na]+ indicating that ESI-MS is useful for the identification of PTX2. Determinations of PTX6 from the toxic phytoplankton and scallops were carried out by LC fluorescence detection. A significantly higher content of PTX6 compared to PTX2 in scallops was observed, suggesting that a transformation of PTX2 to PTX6 in tissues of the scallops occurs rapidly.

摘要

研究了使用非极性柱Sep-Pak C18从海水样品中固相萃取pectenotoxin-2(PTX2)和pectenotoxin-6(PTX6),以测定有毒浮游植物中的PTXs。PTX2和PTX6几乎能从海水样品中完全回收。通过配备大气压电喷雾电离质谱(ESI-MS)的紫外痕量液相色谱(LC)对有毒浮游植物和扇贝中的PTX2进行测定。从有毒浮游植物和扇贝中获得的PTX2产生的质谱显示出丰富的[M+H]+、[M+NH4]+和[M+Na]+,表明ESI-MS可用于PTX2的鉴定。通过LC荧光检测对有毒浮游植物和扇贝中的PTX6进行测定。观察到扇贝中PTX6的含量显著高于PTX2,这表明扇贝组织中PTX2向PTX6的转化迅速发生。

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