UPLC-MS/MS测定水产品中4种麻痹性贝类毒素

Four Paralytic Shellfish Poisonings Determination in Aquatic Products by UPLC-MS / MS Spectrometry

目的建立超高效液相色谱—串联质谱法检测水产品中4种麻痹性贝类毒素的方法。方法贝类样品用0.1 mol/L乙酸超声提取,经亲水亲脂固相萃取小柱净化后,目标物以乙腈(含0.1%甲酸)和乙酸铵(含0.1%甲酸)溶液为流动相,经色谱柱HILIC 150 mm×2.1 mm,3μm梯度洗脱分离,采用电喷雾离子源,多反应监测(MRM)正离子模式进行定性与定量分析,外标法定量。结果各种麻痹性贝类毒素与杂质能良好分离,在各自的线性范围内线性关系良好,相关系数(r)>0.999,方法检测限为10.0μg/kg^31.0μg/kg,在不同浓度水平加标平均回收率(n=6)为81.0%~104%,相对标准偏差(RSD)为0.47%~6.9%。结论本方法前处理方法简单,有较好的灵敏度和重现性,满足水产品中麻痹性贝类毒素的确证和定量分析要求。

Objectives To develop an ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS /MS） method for the determination of four paralytic shellfish poisonings（ PSP） in aquatic products.Methods Samples were ultrasonically extracted by 0. 1mol / L acetic acid,then purified by OASIS HLB solid phase extraction（ SPE）. Four PSPs were separated by HILIC with mobile phase of acetonitrile and ammonium acetate in 0. 1% formic acid. Analytic identification and quantification were performed by electrospray ionization（ ESI）in positive mode using multiple reaction monitoring（ MRM）. Quantification was performed by external standard.Results Four paralytic shellfish poisonings could be separated well from impurities. There was a good linearity in the range of respective working concentration,with a correlation coefficient 0. 999. The limit of quantification was in the range of 10. 0 μg / kg - 31. 0 μg / kg for four PSPs; the average recoveries at different concentration were 81. 0 % - 104 %（ n = 6）,and the relative standard deviations were 0. 47 % - 6. 9 %. Conclusions This method was simple,sensitive and repeatable,which was suitable for the confirmation and quantitative analysis of PSP in shellfish.