摘要
建立了液相色谱-串联质谱分析贝类组织中米氏裸甲藻(GYM)贝毒素、螺环内酯毒素(SPX1)、大田软骨酸(OA)贝毒素、蛤毒素(PTX2)、原多甲藻酸(AZA1)贝毒素的方法。用甲醇-水(4:1,V/V)溶液对贝类组织中GYM,SPX1,OA,PTX2和AZA1进行提取,MAX阴离子交换柱净化后,采用液相色谱分离,除OA以负离子选择反应监测外,GYM,SPX1,PTX2和AZA1以电喷雾离子源正离子选择反应监测模式进行质谱分析。5种脂溶性贝毒素GYM,SPX1,OA,PTX2和AZA1在各自相应浓度范围内线性良好,相关系数>0.99。扇贝闭壳肌空白样品添加5种贝毒素的提取率均为78.6%～94.4%(n=6);精密度(RSD)为6.8%～14.9%。贝类组织中5种贝毒素GYM,SPX1,OA,PTX2和AZA1的检出限分别为0.10,0.21,2.00,0.32和0.04μg/kg。
A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method for the determination of five lipophilic marine toxins including Gymnodimine(GYM),Spirolide-1(SPX1),Okadaic acid(OA) Pecenotoxin-2(PTX2) and Azaspiracid-1(AZA1) in shellfish was developed.After being extracted with methanol and water(80 /20,V/V),the extract was cleaned by solid phase extraction of MAX column,then determined by a reversed phase HPLC gradient program coupled with tandem mass spectrometry in selectedreaction-monitoring mode.GYM,SPX1,OA,PTX2,AZA1were analyzed in positive ion mode,while OA in negative ion mode.The calibration curves were linear well between LC peak area of the selected ion-pair and the concentration of five lipophilic marine toxins with the correlation coefficient over 0.99.The average recoveries from spiked scallop muscle at the concentration ranged from 78.6% to 94.4% with relative standard deviation from 6.8% to 14.9%.The limits of detection were 0.10,0.21,2.00,0.32 and 0.04 μg/kg for GYM,SPX1,OA,PTX2 and AZA1 respectively.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第12期1714-1720,共7页
Chinese Journal of Analytical Chemistry
基金
国家863计划(No.2007AA09Z438)
国家科技支撑计划项目(No.2008BAA94B09)资助
关键词
脂溶性贝毒素
贝类组织
液相色谱-串联质谱
Lipophilic marine toxins
Shellfish
Liquid chromatography-tandem mass spectrometry
