Zhu Li, Tan Wei, Peng Zumao, Deng Mengya, Zhang Xieguang, Yang Guowu
Shenzhen Academy of Metrology and Quality Inspection, Shenzhen 518109, China.
Department of Food and Chemical Engineering, Lushan College of Guangxi University of Science and Technology, Liuzhou 545616, China.
Se Pu. 2017 Sep 8;35(9):949-956. doi: 10.3724/SP.J.1123.2017.05001.
A rapid method was developed for the simultaneous determination of 15 nutrients containing eight vitamin E, six -oryzanols and -carotene in rice by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UHPLC-LTQ/Orbitrap HRMS). The analytes were extracted by methanol containing 0.05% (v/v) 2,6-di-tert-butyl-4-methylphenol (BHT) under the ultrasonic condition, then separated by a Poroshell 120 PFP column (150 mm×3.0 mm, 2.7 μm) with a gradient elution program using 0.1% (v/v) formic acid aqueous solution and methanol containing 0.1% (v/v) formic acid as mobile phases. The detection was performed using an LTQ/Orbitrap HRMS detector with full scan in positive ion mode. Fifteen nutrients were simultaneously separated within 13 min. Furthermore, matrix effects of the white and brown rices were investigated. The correlation coefficients () were ≥ 0.9950 in the linear ranges of the 15 nutrients. The limits of detection (LODs, =3) and limits of quantification (LOQs, =10) of the 15 nutrients were 0.2-1.8 μg/L and 0.7-6.1 μg/L, respectively. At the three spiked levels, the recoveries were 73.2%-101.5% with the relative standard deviations (RSDs) ranging from 1.1% to 5.0% (=3). The method is accurate, efficient and reliable. It is suitable for the simultaneous determination of various nutrients in rice.
建立了一种超高效液相色谱-线性离子阱/轨道阱高分辨质谱(UHPLC-LTQ/Orbitrap HRMS)同时测定大米中15种营养成分(包括8种维生素E、6种谷维素和β-胡萝卜素)的快速方法。样品用含0.05%(v/v)2,6-二叔丁基-4-甲基苯酚(BHT)的甲醇在超声条件下提取,然后采用Poroshell 120 PFP柱(150 mm×3.0 mm,2.7μm),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,通过梯度洗脱程序进行分离。采用LTQ/Orbitrap HRMS检测器在正离子模式下进行全扫描检测。15种营养成分在13分钟内实现了同时分离。此外,还研究了白米和糙米的基质效应。15种营养成分在其线性范围内的相关系数(r)≥0.9950。15种营养成分的检测限(LODs,n = 3)和定量限(LOQs,n = 10)分别为0.2 - 1.8μg/L和0.7 - 6.1μg/L。在三个加标水平下,回收率为73.2% - 101.5%,相对标准偏差(RSDs)为1.1% - 5.0%(n = 3)。该方法准确、高效、可靠,适用于大米中多种营养成分的同时测定。