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超高效液相色谱-串联质谱法同时测定植物油中14种营养成分

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

作者信息

Peng Zumao, Zhu Li, Deng Mengya, Zhang Xieguang, Zheng Yuhui

机构信息

Shenzhen Academy of Metrology and Quality Inspection, National Nutrition Food Testing Center(Guangdong), Shenzhen 518109, China.

出版信息

Se Pu. 2018 Nov 1;36(11):1140-1146. doi: 10.3724/SP.J.1123.2018.07013.

DOI:10.3724/SP.J.1123.2018.07013
PMID:30378377
Abstract

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.

摘要

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。

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