超高效液相色谱-串联质谱法同时快速测定食用油中9种外源性杂质成分

建立了超高效液相色谱-串联质谱同时快速测定食用油中9种外源性杂质成分的分析方法。样品经乙腈涡旋提取后,采用XSelect~?HSS PFP(100 mm×2.1 mm,3.5μm)色谱柱,以5 mmol/L甲酸铵-乙腈为流动相进行梯度洗脱,在10 min内实现9种待测物的良好分离。在电喷雾正离子模式下,以多反应监测(MRM)模式采集数据并作定性鉴别和定量分析。结果表明,9种待测物在相应的质量浓度范围内线性关系良好,相关系数(r^2)均大于0.996;在3个不同浓度加标水平下,平均回收率为68.2%～104%,相对标准偏差(RSD)为2.2%～12%,检出限(LOD,S/N≥3)和定量下限(LOQ,S/N≥10)分别为0.02～0.10μg/kg及0.05～0.25μg/kg。结果表明,该法简单、快速、灵敏、准确、可靠,适用于食用油中9种难挥发外源性特征杂质的同时快速定性和定量分析。

Simultaneous and Rapid Determination of Nine Exogenous Impurities in Edible Oils by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

A comprehensive analytical method was developed and validated for the simultaneous and rapid determination of nine exogenous impurities in edible oils by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS ).The analytes in sample were extracted with acetonitrile using vortex mixer.The chromatographic separation was performed on an XSelect HSS PFP chromatographic column (100 mm×2.1 mm,3.5 μm ),with 5 mmol/L ammonium formate and acetonitrile as mobile phases by gradient elution.The qualitative and quantitative analyses were performed by electrospray ionization mass spectrometry in positive mode under multiple reaction monitoring (MRM ) mode.Results showed that there were good linear relationships for nine analytes in corresponding concentration range with their correlation coefficients ( r 2 ) larger than 0.996.Average recoveries for 9 analytes in sample at three spiked levels ranged from 68.2 % to 104 %,with relative standard deviations (RSD ) of 2.2 %-12 %.The limits of detection (LOD, S/N ≥3 ) and quantitation (LOQ, S/N ≥10 ) were in the ranges of 0.02-0.10 μg/kg and 0.05-0.25 μg/kg,respectively.The established method is simple,rapid,sensitive,accurate and reliable,and is suitable for the simultaneous and rapid determination of nine exogenous characteristic impurities in edible oils.