高效液相色谱-串联质谱法同时测定食用油中的16种抗氧化剂

利用高效液相色谱-串联质谱(HPLC-MS/MS)同时测定食用油中16种抗氧化剂。食用油中的抗氧化剂经正己烷溶解、含L-抗坏血酸棕榈酸盐的乙腈萃取后,经C18柱分离,乙腈-0.1%甲酸溶液体系为流动相进行梯度洗脱,多反应监测模式(MRM)检测,外标法定量。16种抗氧化剂呈良好的线性关系(r~2=0.9912~0.9988),方法的测定低限为0.1~0.5mg/kg,在测定低限浓度水平下的平均回收率为78.6%~101.2%,相对标准偏差为3.50%~13.19%(n=10)。该方法准确、灵敏、重现性好,可用于食用油中16种抗氧化剂的检测。

Simultaneous Determination of 16 Antioxidants in Edible Oil Using High Performance Liquid Chromatography--Electrospray Ionization Tandem Mass Spectrometry

A method was developed for the simultaneous determination of 16 antioxidants in edible oil using high performance liquid chromatography-tandem mass spectrometry. The antioxidants in the sample were dissolved with hexane, extracted with acetonitrile containing ascorbyl palpitate, separated on a reversed-phase C18 column with a mobile phase of acetonitrile-water containing 0.1%formic acid by gradient elution. The detection was performed by MS/MS under multiple reaction monitoring（MRM）mode, and the quantitation was carried out by the external standard method. The calibration curves showed good linearities for 16 antioxidants with correlation coefficients of 0.991 2-0.998 8. The determination limits of 16 antioxidants were between 0.1 mg/kg and 0.5 mg/kg. Sample were fortifid at the level of the limit of determination with the antioxidants mixed standard solution. The recoveries were between 78.6%and 101.2%, and the relative standard deviations of repeatability were between 3.50%and 13.19%（n=10）. The method is reliable, sensitive and reproducible, and can be applied in the determination of 16 antioxidants in edible oil.