超高效液相色谱-串联质谱法同步测定贝类水产品中4种脂溶性藻毒素

Simultaneous determination of 4 types of lipophilic algae toxins in shellfish products using ultra performance liquid chromatography tandem mass spectrometry

目的建立一种超高效液相色谱-串联质谱法同时测定贝类产品中4种脂溶性藻毒的方法。方法样品采用甲醇均质提取,用HLB小柱净化,在乙腈-5 mmol/L醋酸铵水溶液体系中,经Kinetex C18柱(150 mm×3 mm,2.6μm)梯度洗脱,实现了4种藻毒素的良好分离。采用了电喷雾正负离子同时监测模式对4种脂溶性藻毒素进行外标法定量测定。结果目标化合物的检出限为2.3~20.7 pg/g,在3.8~1378.0 pg/g浓度范围内线性良好,相关系数r^2在0.99407-0.99923之间,同时以贝类产品为基底的4种化合物在高、中、低3个加标水平浓度下的回收率为70%~95%,相对标准偏差(relative standard deviation,RSD)为2.3%~7.7%。结论该方法灵敏、准确、高效,适合用于贝类水产品食用安全的日常风险监测项目中。

Objective To establish a method for simultaneous determination of 4 kinds of lipophilic algae toxins in shellfish products using ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Methods Samples were first extracted by methanol,followed by a purification using an Oasis HLB SPE column.Further separation of the 4 targets compound was achieved on a Kinetex C18 column(150 mm×3 mm,2.6μm)via UPLC by gradient elution with acetonitrile and 5 mmol/L ammonium acetate aqueous solutionas mobile phase.Quantification of the 4 targets was performed on a mass spectrometry,which simultaneously carried out by means of electrospray ionization in positive(ESI+)and negative ion mode(ESI-)mode with an external standard.Results The method showed a good linearity in the concentration range of 3.8-1378.0 pg/g,with the detection limits of2.3-20.7 pg/g.The correlation coefficients(r^2)were between 0.99407-0.99923 for 4 toxins.The average recoveries for the high,medium and low concentrations of external standard were between 70%-95%with the relative standard deviations(RSD)2.3%-7.7%.Conclusion The method is sensitive,accurate,with high efficiency and is suitable for the daily risk monitoring project of shellfish food safety.