液相色谱-串联质谱法检测贝类产品中麻痹性贝类毒素

Determination of Paralytic Shellfish Poisoning Toxins in Shellfish by Liquid Chromatography with Tandem Mass Spectrometry

建立了贝类组织中11种麻痹性贝类毒素的高效液相色谱-串联质谱分析方法,包括STX、dcSTX、NEO、dcNEO、GTX1-4、dcGTX2,3和GTX5(B1)。贝类样品经含0.1%甲酸的80%(体积分数)乙腈水溶液超声提取后,经过冷冻分层,下层固体融化后通过HLB固相萃取小柱富集净化和10 000MWCO(Molecular Weight Cutoff)超滤管超滤截留,超滤液用于仪器分析。采用Zwitterionic亲水性相互作用色谱柱(250 mm×4.6 mm,5μm,德国)分离,在多反应监测模式下进行定性和定量分析。各组分在一定的范围内具有良好的线性关系,平均回收率大于60%,相对标准偏差小于20%(n=7)。用该方法分析染毒的栉孔扇贝样品,证实了对PSP毒素具有良好的分析测定效果。

A liquid chromatography-electrospray ionization triple-quadruple tandem mass spectrometric method has been established for the determination of eleven kinds of paralytic shellfish poisoning toxins including STX, dcSTX, NEO, dcNEO, GTX1 - 4, deGTX2,3 and GTX5 （B1）. After being extracted using aeetonitrile and water （80：20,V/V） including 0.1% formic acid, the solution was frozen to separate into two layers. To melt the solid, then the solution would be cleaned-up by solid phase extraction （SPE） on an Oasis HLB cartridge. In order to get rid of macromolecule compound, the sample was ultra filtrated with 10 000 MWCO（ Molecular Weight Cutoff） ultra-filtration device. The ultra-filtration solution would be analyzed. The sample would be separated on a Zwitterionic hydrophilic interaction liquid chromatography column （250 mm × 4. 6 mm,5 μm）. The quantitative and confirmatory determinations of PSP were performed by multiple reactions monitoring mode. All components showed good linear relation in the suitable range. The mean recoveries were more than 60% and the relative standard deviations were less than 20% （n = 7）. The method has been applied to the analysis of samples contaminated with PSP toxins with satisfactory result.