Mass spectrometric screening method for microcystins in cyanobacteria

被引：80

作者：

Harada, K ^{[1
]}

Murata, H ^{[1
]}

Qiang, Z ^{[1
]}

Suzuki, M ^{[1
]}

Kondo, F ^{[1
]}

机构：

[1] AICHI PREFECTURAL INST PUBL HLTH, KITA KU, NAGOYA, AICHI 462, JAPAN

来源：

TOXICON | 1996年 / 34卷 / 06期

关键词：

D O I：

10.1016/0041-0101(95)00163-8

中图分类号：

R9 [药学];

学科分类号：

1007 ;

摘要：

A screening method for microcystins in cyanobacteria, which consists of the formation of 3-methoxy-2-methyl-4-phenylbutyric acid as an oxidation product of microcystins by ozonolysis, and detection of 3-methoxy-2-methyl-4-phenylbutyric acid by thermospray-liquid chromatography/mass spectrometry or electron ionization-gas chromatography/mass spectrometry using selected ion monitoring, was developed. The ozonolysis made it possible to significantly reduce the formation times of 3-methoxy-2methyl-4-phenylbutyric acid because the previously required extraction, clean-up and other procedures could be entirely eliminated. The resulting intact 2-methyl-4-phenylbutyric acid was directly analyzed by thermospray-liquid or electron ionization-gas chromatography/mass spectrometry, and the procedures from ozonolysis to analysis of microcystins at the pmole levels were performed within only 30 min. The calibration curves obtained by thermospray-liquid or electron ionization-gas chromatography/mass spectrometry analysis showed a linear relationship from 14 to 830 pmole and from 2.5 to 100 pmole of microcystin-LR, respectively. The method was applied to the detection and determination of the total amount of microcystins in bloom and cultured samples, showing that it provided a means of not only screening for microcystins but of their accurate quantitation. Copyright (C) 1996 Elsevier Science Ltd

引用

页码：701 / 710

页数：10

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