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目的采用超高效液相色谱-串联质谱法建立贝类产品中AZA1、AZA2、AZA3、OA、DTX1、DTX2多种毒素的定性、定量检测方法。方法贝类样品用甲醇提取后,Strata-X固相萃取柱净化。采用ACQUITY UPLCTMBEH C18(2.1 mm×50 mm,1.7μm)色谱柱分离,多反应监测模式(MRM)对目标化合物定性及定量分析。结果所检测的贝类毒素线性相关系数均大于0.998;方法定量下限(LOD)为0.05μg/kg~0.8μg/kg;高、中、低3个添加水平的平均加标回收率在85.6%~96.7%之间,相对标准偏差为3.6%~11.4%。结论该方法灵敏度高、操作简单高效,适用于贝类水产品中原多甲藻酸毒素和大田软海绵酸贝类毒素的同时检测分析。
OBJECTIVE To establish a qualitative and quantitative method for the determination of AZA1, AZA2, AZA3, OA, DTX1 and DTX2 toxins in shellfish by ultra performance liquid chromatography-tandem mass spectrometry. Methods Shellfish samples were extracted with methanol and purified using Strata-X SPE cartridges. The target compounds were characterized and quantified using an ACQUITY UPLC TMBEH C18 (2.1 mm × 50 mm, 1.7 μm) column with multiple reaction monitoring (MRM). Results The linear correlation coefficients of tested shellfish toxins were all greater than 0.998. The LOD of the method was 0.05μg / kg ~ 0.8μg / kg. The average recoveries of three high, medium and low levels were between 85.6% 96.7%, the relative standard deviation was 3.6% ~ 11.4%. Conclusion The method has high sensitivity, simple and high efficiency and is suitable for the simultaneous detection and analysis of protocatechuic acid and megesofluidic acid toxin in shellfish aquatic products.