液质联用法测定植物油中的4种没食子酸酯

Determination of Gallates in Vegetable Oil by UPLC-MS/MS

建立了食用植物油中没食子酸酯类化合物测定的超高效液相色谱-串联质谱分析方法。样品经正己烷饱和的乙睛萃取后,采用ACQUITY UPLC HSS T3色谱柱分离,以0.1%甲酸水和甲醇为流动相梯度洗脱,电喷雾电离负离子模式下多反应监测(MRM)模式进行定性、定量检测。4种没食子酸酯类化合物的检出限(S/N=3)为0.02 mg/kg^0.05 mg/kg,定量限(S/N=10)为0.06 mg/kg^0.15 mg/kg;在0.20、0.50、0.80 mg/kg 3个加标水平下回收率为75.4%~91.3%,相对标准偏差小于9.2%。应用建立的方法对市售食用植物油产品进行测定,未发现4种没食子酸酯类化合物。

A method was established for the determination of gallates in edible vegetable oil based on ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The oil sample was extracted by hexane-saturated acetonitrile, and the chromatographic separation was performed on an ACQUITY UPLCTM HSS T3 column（2.1 mm×50 mm,1.7 μm） by gradient elution with 0.1 % formic acid solution and methanol as the mobile phase. The analyte was detected by electrospray ionization in negative ion mode-MS/MS in multiple reaction monitoring（MRM） mode. For the four gallates, the limits of detection（LOD） were from 0.02 mg/kg to 0.05 mg/kg and the limits of quantification（LOQ） were from 0.06 mg/kg to 0.15 mg/kg. The average recoveries were ranged from 75.4 % to 91.3 % at the spiked levels of 0.20,0.50,0.80 mg/kg, with the relative standard deviations（RSDs） were not more than 9.2 %. Some edible vegetable oil products from local market were detected by the developed method, and the four gallates were not found.