Peng Zumao, Zhu Li, Deng Mengya, Zhang Xieguang, Zheng Yuhui
Shenzhen Academy of Metrology and Quality Inspection, National Nutrition Food Testing Center(Guangdong), Shenzhen 518109, China.
Se Pu. 2018 Nov 1;36(11):1140-1146. doi: 10.3724/SP.J.1123.2018.07013.
A method for the simultaneous determination of four tocopherols, four tocotrienols, four phytosterols, -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 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 () 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.
建立了一种超高效液相色谱 - 串联质谱法(UHPLC - MS/MS)同时测定四种生育酚、四种生育三烯酚、四种植物甾醇、β - 胡萝卜素和角鲨烯的方法。皂化后,样品用石油醚萃取,萃取液经旋转蒸发浓缩。残渣在氮气气氛下干燥,并用甲醇溶解。14种营养成分在Poroshell 120 PFP柱(150 mm×3.0 mm,2.7μm)上分离,以0.1%(v/v)甲酸水溶液和含0.1%(v/v)甲酸的甲醇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(APCI)质谱仪,在正模式下进行选择性反应监测(SRM)检测。14种营养成分在0.05 - 10.0 mg/L范围内呈线性,相关系数(r)不小于0.9971。植物油样品中14种营养成分在三个加标水平下的平均回收率为80.7%至100.5%,相对标准偏差(RSDs)小于6.0%。检测限(LODs)范围为0.01至0.30μg/g。定量限(LOQs)在0.04 - 1.00μg/g范围内。该方法灵敏、准确、快速且稳定,适用于植物油样品中14种营养成分的同时测定。