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目的利用高效液相色谱-串联质谱法(HPLC-MS/MS)建立同时测定水产品11种麻痹性贝类毒素的快速分析方法。方法采用乙酸(0.1mol/L)提取贝类或鱼类中的麻痹性贝类毒素,经OASIS HLB固相萃取小柱净化后,以乙腈-乙酸铵溶液作为流动相,液相色谱柱分离,通过改变乙腈在流动相中的比例和流速,采用HPLC/MS/MS电喷雾电离(ESI),阳离子模式,多反应监测(MRM)方式检测,外标法定量。结果 11种PSP在不同浓度下的平均加标回收率为90.7%～96.2%,线性相关系数均大于0.998,相对标准偏差(RSD)均小于9.3%,定量检出限在0.12～0.24ng/g。结论 HPLC-MS/MS法操作简便,灵敏度、精密度高,重现性较好,对水产品中痕量麻痹性贝类毒素具有良好的分析效果。
OBJECTIVE To establish a rapid method for simultaneous determination of 11 paralytic shellfish toxins in aquatic products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods Paralytic shellfish toxins from shellfish or fish were extracted with acetic acid (0.1mol / L), purified by OASIS HLB cartridge, eluted with acetonitrile-ammonium acetate solution as mobile phase and separated by liquid chromatography. By changing the proportion of acetonitrile in the mobile phase and the flow rate, HPLC / MS / MS electrospray ionization (ESI), cation mode, multiple reaction monitoring (MRM) Results The average recoveries of 11 PSPs ranged from 90.7% to 96.2% with linear correlation coefficients greater than 0.998. The relative standard deviations (RSDs) were all less than 9.3%. The detection limits were between 0.12 and 0.24 ng / g . Conclusion HPLC-MS / MS method has the advantages of simple operation, high sensitivity, high precision and good reproducibility. It has good analytical value for trace paralytic shellfish toxins in aquatic products.