高效液相色谱-串联质谱法同时测定酒中6种对羟基苯甲酸酯类防腐剂

Simultaneous Determination of 6 Parabens in Wine by High Performance Liquid Chromatography Tandem Mass Spectrometry

建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)同时测定酒中6种对羟基苯甲酸酯类防腐剂的分析方法。试样用乙酸乙酯提取,经Poroshell 120 EC-C18色谱柱(2.1 mm×75 mm, 2.7 μm)进行分离,在电喷雾电离(electrospray ionization source,ESI)源负离子模式下,进行多反应监测(multiple reaction monitoring,MRM)。6种对羟基苯甲酸酯在5 ng/mL^2 000 ng/mL的浓度范围内线性关系良好,相关系数r2 >0.999,在低、中、高3个加标浓度水平下的平均回收率为79.1 %~107.5 %,相对标准偏差(relative standard deviation,RSD)为1.1 %~9.1 %(n=7)。方法检出限(limit of detection,LOD)为0.8 μg/kg^1.0 μg/kg,定量限(limits of quantitation,LOQ)为3.1 μg/kg ~3.6 μg/kg。

A method was developed for the simultaneous determination of 6 parabens in wine by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were extracted by ethyl acetate, separated on a Poroshell 120 EC-C18 column (2.1mm × 75 mm, 2.7 μm), and determined with negative ion mode of electrospray ionization (ESI) under multiple reaction monitoring (MRM) mode. The calibration curves of 6 parabens were linear in the range of 5 ng/mL -2 000 ng/mL with good correlation coeffi-cients (r2 >0.999). The average recoveries at the three different spiked concentrations were 79.1.%-107.5 % with relative standard deviations (RSDs, n = 7) of 1.1 %-9.1 %. The limits of detection and quantitation of the method were 0.8 μg/kg-1.0 μg/kg and 3.1 μg/kg-3.6 μg/kg, respectively.