建立了QuEChERS净化技术结合高效液相色谱-串联质谱法测定食用贝类产品中4种脂溶性贝类毒素(OA,SPX1，DTX1,AZA1)的快速方法。贝类样品匀质后用85%乙腈水萃取，采用QuEChERS净化技术对其进行富集净化后，用HPLC-MS/MS进行检测。以乙腈-水溶液(2 mmo/L乙酸铵，0.1%甲酸）为流动相进行梯度洗脱，经C18色谱柱分离，在多反应监测(MRM)模式下扫描。采用标准曲线外标法定量，OA和DTX1的方法检出限为10 μg/kg，在1.0~100 μg/L范围内线性关系良好；AZA1和SPX1的方法检出限为1.0 μg/kg，在1.0~20 μg/L范围内线性关系良好，相关系数(r2)均大于0.999。高、中、低三个添加水平的平均回收率在81.9%~93.1%之间，RSD小于5%。应用该方法对进出口的贻贝、北极贝、象拔蚌、牡蛎等15个样品进行检测，发现5个样品的SPX1测定结果为阳性。该方法操作简便、灵敏度高、重现性好，适用于贝类产品中脂溶性贝类毒素的检测。

A novel method was developed to detect four lipophilic shellfish toxins (OA, SPX1, DTX1, and AZA1) in edible shellfish products via a combination of QuEChERS technology and high performance liquid chromatography-tandem Mass Spectrometry (HPLC- MS/MS). The samples were homogeneously extracted with acetonitrile-water (85%, V/V) and purified with QuEChERS technology. Using C18 column with acetonitrile/water (2 mmol/L ammonium acetate, 0.1% formic acid) as mobile phase, the analytes were separated by HPLC-MS/MS with electrospray ionization (ESI) mode, followed by multiple reaction monitoring (MRM). Quantification was performed by external standard calibration method．The limits of detection (LOD, S/N=3) for OA and DTX1 were 10 μg/kg, the calibration curves showed good linearity in the range of 1.0 to 100 μg/L, while the LOD for AZA1 and SPX1 was 1.0 μg/kg, with a linearity range between 1.0 20 μg/L. The correlation coefficients (r2) were > 0.999 for all four toxins. The average spiked recoveries of the shellfish toxins at three concentration levels were between 81.9% and 93.1% while relative standard deviation (RSD) was < 5%. A total of 15 import and export samples of fish including mussels, octopus, geoducks, and oysters were screened by this newly developed method and SPX1 toxin was found in 5 samples. This method is quick, easy-to-perform, sensitive, and appropriate to detect lipophilic shellfish toxins in shellfish products.

广东检验检疫局科技计划项目（2012GDK38）；国家质检总局科技计划项目（2011k193)