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目的:建立固相萃取、高效液相色谱串联质谱法测定贝类产品中AZA1、YTX、OA、PTX2、GYM、SPX1、DTX-1 7种脂溶性贝类毒素残留的方法。方法:贝类样品用甲醇提取后,Strata-X固相萃取柱净化,甲醇洗脱。采用Waters Sun-FireTMC18(100 mm×2.1 mm,3.5μm)色谱柱,以乙腈-2 mmol/L乙酸铵水(80:20,v/v)作为流动相,流速0.2 ml/min,采用电喷雾质谱电离,多反应监测模式(MRM)对目标化合物定性及定量分析,外标法定量。结果:7种贝类毒素线性相关系数均大于0.998;方法定量下限(LOQ)为0.1μg/kg~2.7μg/kg;高、中、低3个添加水平的平均加标回收率在72.2%~101.9%,相对标准偏差为2.0%~13.6%。结论:该方法灵敏度高、操作简单高效,适用于贝类样品中脂溶性贝类毒素的定量及确证分析。
OBJECTIVE: To establish a method for the determination of 7 kinds of liposoluble molluscicides residues in shellfish products by solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry. Methods: After the shellfish samples were extracted with methanol, the Strata-X SPE cartridge was cleaned up and eluted with methanol. The mobile phase was eluted with a Waters Sun-Fire TMC18 (100 mm × 2.1 mm, 3.5 μm) column with acetonitrile-2 mmol / L ammonium acetate in water (80:20, v / v) Mass spectrometry ionization, multiple reaction monitoring mode (MRM) of the target compound qualitative and quantitative analysis, external standard quantitative. Results: The linear correlation coefficients of seven kinds of shellfish toxins were all greater than 0.998. The LOQ was 0.1μg / kg ~ 2.7μg / kg. The average recoveries of three high, medium and low levels were between 72.2% 101.9% with relative standard deviation of 2.0% ~ 13.6%. Conclusion: The method is sensitive, simple and efficient, and suitable for the quantitative and confirmatory analysis of liposoluble shellfish toxins in shellfish samples.