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建立了Qu ECh ERS净化技术结合高效液相色谱-高分辨飞行时间质谱法测定食用贝类产品中4种脂溶性贝类毒素(Okadaic Acid,OA、Spirolides1,SPX1、Dinophysistoxin1,DTX1、Azaspiracid1,AZA1)的快速方法。以Qu ECh ERS净化技术对食用贝类样品进行提取与净化后,经C18色谱柱分离,用高分辨飞行时间质谱仪(ESI源)进行测定。用Peak View软件对分析结果进行全智能分析,对照每个样品与标准品的TOF-MS质量精度及同位素分布情况、保留时间以及TOF-MS/MS谱图,对化合物作出定性判断。同时利用Multi Quant软件对四种毒素进行外标法定量,OA和DTX1的线性范围为2.0~100μg/L,方法检出限为10μg/kg;AZA1和SPX1的线性范围为0.5~20μg/L,方法检出限为2.0μg/kg,相关系数(R2)均大于0.997。高、中、低三个添加水平的平均回收率在75.6%~94.1%之间,RSD小于10%。应用该方法对进出口的贻贝、北极贝、象拔蚌、牡蛎等20个样品进行检测,发现8个样品的SPX1和2个AZA1测定结果为阳性。该方法操作简便、高效快速、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 set of Qu ECh ERS purification technology and high performance liquid chromatography-high resolution liquid chromatography-time of flight mass spectrometry were established for the determination of four kinds of fat-soluble shellfish toxins (Okadaic Acid, OA, Spirolides1, SPX1, Dinophysistoxin1, DTX1, Azaspiracid1, AZA1) Fast method Edible shellfish samples were extracted and purified using the Qu ECh ERS purification technique and then separated on a C18 column using a high resolution time of flight mass spectrometer (ESI source). Peak View software was used to analyze the analysis results intelligently. The quality of TOF-MS, isotope distribution, retention time and TOF-MS / MS spectra of each sample and standard were compared qualitatively. At the same time, the four toxins were quantified by external standard method with Multi Quant software. The linear range of OA and DTX1 was 2.0 ~ 100μg / L and the detection limit was 10μg / kg. The linear range of AZA1 and SPX1 was 0.5 ~ 20μg / L, The detection limit was 2.0μg / kg, and the correlation coefficient (R2) was greater than 0.997. The average recoveries of three high, medium and low levels were between 75.6% and 94.1% with RSD less than 10%. Using this method, 20 samples of imported and exported mussels, Arctic sea buckthorn, geoduck, and oyster were tested and found that SPX1 and 2 AZA1 of 8 samples were positive. The method has the advantages of simple operation, high efficiency, high sensitivity and good reproducibility, and is suitable for the detection of fat-soluble shellfish toxins in shellfish products.