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

Simultaneous determination of 14 nutrients in vegetable oils by ultra high performance liquid chromatographytandem mass spectrometry

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. 7μm)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. 997 1;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. 30μg/g和0. 04～1. 00μg/g。该法灵敏、准确,分析时间快,稳定性好。

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 N 2 atmosphere and dissolved with methanol.The 14 nutrients were separated on a Poroshell 120 PFP column(150 mm×3.0 mm,2.7μm)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 0.997 1.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 0.30μg/g.The limits of quantification(LOQs)were in the range of 0.04-1.00μg/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.