Simultaneous determination of biotoxins DSP and AZAs in bivalve molluscs and fish by liquid chromatography/tandem mass spectrometry
Simultaneous determination of biotoxins DSP and AZAs in bivalve molluscs and fish by liquid chromatography/tandem mass spectrometry
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液相色谱/串联质谱法同时测定双壳类软体动物和鱼类中的生物毒素DSP和AZA
DOI：
10.1002/rcm.6900
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发表时间：
2014
影响因子：
2
通讯作者：
Chen G.
中科院分区：
文献类型：
--
作者：
Zhuo L.;Fu W.;Yang Y.;Qiu B.;Lin Z.;Shan L.;Zheng L.;Li J.;Chen G.
建立了一种同时测定水产品中毒素OA、DtX-1、AZA-1、AZA-2和AZA-3的方法。方法采用C18色谱柱(150 mm × 2.1 mm，3.5 µm)，乙腈/水梯度洗脱，甲酸为洗脱改进剂。对于OA和DTX-1，负电喷雾电离(ESI)用于产生分子相关离子[M-H]-，而对于AZAS，电喷雾电离(ESI)用于产生分子相关离子[M+H]+。样品经80%甲醇提取、乙酸乙酯分配、Poly-Sery Max色谱柱净化后，采用LC/ESI-MS/MS多反应监测模式进行分析。结果该方法的检出限为0.02~0.79 µg/kg，定性限为0.07~2.64 µg/kg。三个添加水平的回收率为71.3%~104.8%，相对标准偏差为1.0%~12.5%。所选离子对的LC峰面积与毒素浓度呈良好的线性关系，相关系数均在0.99以上。结论该方法灵敏度高，可用于水产品中毒素DSP和AZA的测定。版权所有©2014 John Wiley&Sons，Ltd.
RATIONALEA method has been developed for simultaneous determination of the toxins OA, DTX‐1, AZA‐1, AZA‐2 and AZA‐3 in various aquatic products as these can cause diarrhoetic shellfish poisoning (DSP) in humans, an intoxication characterized by vomiting and diarrhea.METHODSSeparation of the toxins was achieved on a C18 column (150 mm × 2.1 mm, 3.5 µm) using an acetonitrile/water gradient with formic acid as an eluent modifier. Electrospray ionisation (ESI) in negative mode was used to generate the molecule related ion [M–H]–, for OA and DTX‐1, while ESI in positive mode was used to generate the molecule related ion [M+H]+for AZAs. Samples were extracted with 80% methanol, followed by partitioning with ethyl acetate, purified on a Poly‐Sery MAX cartridge and finally analyzed by LC/ESI‐MS/MS in the multiple reaction monitoring (MRM) mode.RESULTSThe limit of detection (LOD) and limit of qualification (LOQ) of the method were in the range of 0.02–0.79 µg/kg and 0.07–2.64 µg/kg inScomberomorus niphonius, blood clam and oyster, respectively, recoveries of the toxins at three fortification levels ranged from 71.3% to 104.8% with relative standard deviation from 1.0% to 12.5%. The calibration curves were well linear between the LC peak area of the selected ion pair and the concentration of the toxins, with the correlation coefficient over 0.99.CONCLUSIONSThe method was sufficiently sensitive to permit the determination of the toxins DSP and AZA in sea food. Copyright © 2014 John Wiley & Sons, Ltd.