固相萃取-液相色谱-串联质谱法测定海产品中谷氨酸钠的含量

Determination of Sodium Glutamate in Seafood by Solid-phase Extraction-Gas Chromatography-Tandem Mass Spectrometry

目的:建立海产品中谷氨酸钠的固相萃取-液相色谱-串联质谱法测定方法。方法:样品经盐酸水溶液提取、离心、过滤、MAX固相萃取柱净化后,以含0.2%甲酸乙腈溶液-0.2%甲酸水溶液为流动相,梯度洗脱,经Agilent PFP色谱柱(2.1 mm×100 mm,2.7μm)分离后,采用四极杆串联质谱仪电喷雾正离子模式和多反应监测(MRM)模式进行检测。结果:谷氨酸钠在测定范围内相关系数为0.9998。仪器检出限为1.5μg/L,定量限为5.0μg/L,平均加标回收率为97.9%,相对标准偏差(RSD)为1.2%。结论:该方法具有灵敏、准确的特点,适用于海产品中谷氨酸钠的测定。

Objective:To establish a method for the determination of sodium glutamate in seafood by solid-phase extraction-gas chromatography-tandem mass spectrometry.Method:Samples are extracted by hydrochloric acid aqueous solution,centrifuged,filtered and purified by MAX solid-phase extraction column.The aqueous solution containing-0.2%formic acid and 0.2%formic acid and acetonitrile is purified by gradient elution and separated by Agilent PFP column(2.1 mm×100 mm,2.7μm).The quadrupole tandem mass spectrometry(ESI)is used to electrospray positive ion mode and multiple reactions monitoring(MRM)mode is used for detection.Results:The correlation coefficient of sodium glutamate in the determination range is 0.9998.The detection limit is 1.5μg/L and the quantitative limit is 5.0μg/L,the average recovery rate is 97.9%,and the relative standard deviation(RSD)is 1.2%.Conclusion:The method is sensitive and accurate and it is suitable for the determination of sodium glutamate in seafood.