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超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱快速测定大米中15种营养成分 被引量:7

Rapid determination of 15 nutrients in rice by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry
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摘要 建立了超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(UHPLC-LTQ/Orbitrap HRMS)同时快速检测大米中15种营养成分(8种维生素E、6种γ-谷维素及β-胡萝卜素)的方法。样品经过含0.05%(v/v)2,6-二叔丁基-4-甲基苯酚(BHT)的甲醇溶液超声提取处理后,用Poroshell 120 PFP色谱柱(150 mm×3.0 mm,2.7μm)分离,以0.1%(v/v)甲酸水溶液和含0.1%(v/v)甲酸的甲醇溶液为流动相,在正离子模式下通过UHPLC-LTQ/Orbitrap HRMS进行全扫描分析。15种营养成分可在13 min内获得满意的分离效果。15种营养成分在各自的线性范围内线性关系良好,相关系数(r)≥0.995 0,15种营养成分的检出限(S/N=3)为0.2~1.8μg/L,定量限(S/N=10)为0.7~6.1μg/L,在3个添加水平下的平均加标回收率分别为73.2%~101.5%,相对标准偏差(RSD)为1.1%~5.0%(n=3)。该法准确,高效,可靠,适用于大米中多种营养成分的同时测定。 A rapid method was developed for the simultaneous determination of 15 nutrients containing eight vitamin E,six y-oryzanols and 6-carotene in rice by ultra high performance liq-uid chromatography-linear ion traorbitrap 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 mmx3. 0 mm,2. 7 pm) 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 pha-ses. The detection was performed using an LT Orbitrap HRMS detector with full scan in posi-tive ion mode. Fifteen nutrients were simultaneously separated within 13 min. Furthermore, matrix effects of the white and brown rices were investigated. The correlation coefficients (r ) were0. 995 0 in the linear ranges of the 15 nutrients. The limits of detection (LODs, S/N =3) and limits of quantification (LOQs, S/N = 10) of the 15 nutrients were 0. 2-1. 8 μL and 0. 7 -6. 1 pg/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% ( n = 3). The method isaccurate, efficient and reliable. It is suitable for the simultaneous determination of various nutrients in rice.
出处 《色谱》 CAS CSCD 北大核心 2017年第9期949-956,共8页 Chinese Journal of Chromatography
基金 广东省质量技术监督局科技项目(2017CZ12)~~
关键词 超高效液相色谱 线性离子阱/静电场轨道阱高分辨质谱 营养成分 维生素E γ-谷维素 6-胡萝卜素 大米 ultra high performance liquid chromatography (UHPLC) linear ion trap-orbitrap high resolution mass spectrometer (LTQ/Orbitrap HRMS) nutrients vitamin E γ-oryzanol β-carotene rice
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