高效液相色谱-串联质谱联用测定水产品中麻痹性贝类毒素

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。

Determination of paralytic shellfish toxins in aquatic products by high performance liquid chromatography coupled with electrospray tandem mass spectrometry

Objective To establish a method for determination of 11 paralytic shellfish toxins in aquatic products simultaneously by high performance liquid chromatography coupled with electrospray tandem mass spectrometry. Methods Homogenized food samples were socked in 0.1 mol/L HAc and ultrasonically extracted for 15 minutes,and cleaned up by solid phase extraction of OASIS HLB column.High performance liquid chromatography-tandem mass spectrometric method was used to determinate 11 paralytic shellfish toxins,which were separated by HILIC with mobile phase of acetonitrile and ammonium acetate.Analyte identification and quantification were performed by electrospray ionization（ESI） in positive mode using multiple reaction monitoring. Results The correlation coefficients of calibration curve were above 0.998.The detection limits of the method were 0.12~ 0.24ng/g（S/N=10）.The spiked recoveries ranged from 90.7% to 96.2%（n=7）.And the relative standard derivations were lower than 9.3%. Conclusion The method was simple,effective,and accurate an suitable for determination of paralytic shellfish toxin in aquatic products.