超高效液相色谱-串联质谱同时测定植物油中14种营养成分

建立超高效液相色谱-串联质谱同时检测植物油中4种生育酚、4种生育三烯酚、4种植物甾醇、β-胡萝卜素和角鲨烯等14种营养成分的方法。样品经皂化处理后，采用石油醚提取浓缩，用甲醇定容。采用Poroshell 120 PFP色谱柱（150 mm×3.0 mm，2.7 μm）分离，以0.1%（v/v）甲酸水溶液和0.1%（v/v）甲酸甲醇溶液为流动相进行梯度洗脱，流速为0.3 mL/min。采用大气压化学电离源、正离子模式，在选择反应监测模式下扫描。结果表明，14种营养成分在0.05~10.0 mg/L范围内相关系数≥0.9971；在不同添加水平下，14种营养成分的回收率为80.7%~100.5%，相对标准偏差＜6.0%（n=6）；方法的检出限和定量限分别为0.01~0.30 μg/g和0.04~1.00 μg/g。该法灵敏、准确，分析时间快，稳定性好，适用于植物油中14种营养成分的同时检测。

Simultaneous determination of 14 nutrients in vegetable oils by ultra high performance liquid chromatography-tandem mass spectrometry

A method for the simultaneous determination of four tocopherols, four tocotrienols, four phytosterols, β-carotene and squalene by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed. After saponification, the samples were extracted with petroleum ether, and the extract solution was concentrated by rotary evaporation. The residue was dried under a N₂ atmosphere and dissolved with methanol. The 14 nutrients were separated on a Poroshell 120 PFP column (150 mm×3.0 mm, 2.7 μm) by gradient elution with 0.1% (v/v) formic acid aqueous solution and methanol containing 0.1%(v/v) formic acid as the mobile phases at a flow rate of 0.3 mL/min. The detection was performed using an atmospheric pressure chemical ionization (APCI)-mass spectrometer with selective reaction monitoring (SRM) in positive mode. The results were linear in the range of 0.05-10.0 mg/L for the 14 nutrients, and the correlation coefficients (r) were no less than 0.9971. The average recoveries of the 14 nutrients in the vegetable oil samples ranged from 80.7% to 100.5% at three spiked levels, and the relative standard deviations (RSDs) were less than 6.0%. The limits of detection (LODs) ranged from 0.01 to 0.30 μg/g. The limits of quantification (LOQs) were in the range of 0.04-1.00 μg/g. The proposed method is sensitive, accurate, fast and stable, and is suitable for the simultaneous determination of the 14 nutrients in vegetable oil samples.