数字农科院2.0

Determination of Nicotinamide in Rice by Pre-column Derivatization and High Performance Liquid Chromatography-Mass Spectrometry

文献类型: 外文期刊

作者: Cao Zhao-Yun;Mou Ren-Xiang;Chen Ming-Xue

作者机构:

关键词: Nicotinamide;rice;pre-column derivatization;liquid chromatography-mass spectrometry

期刊名称: CHINESE JOURNAL OF ANALYTICAL CHEMISTRY

ISSN: 0253-3820

年卷期: 2009 年 37 卷 7 期

页码:

收录情况: SCI

摘要: A method was developed for the determination of nicotinamide (NA) in rice by pre-column derivatization and high performance liquid chromatography/electrospray ionization mass spectrometry (HPLC/ESI-MS). After extraction with water, NA was derivatized by 9-fluorenylmethoxycarbonyl (FMOC-CI). In order to enhance the sensitivity, the derivatization was optimized regarding organic solvent content and amount of FMOC-Cl. The best HPLC conditions for the separation of NA in real samples were achieved using a C(18) column and mobile phase which contained 0.1% formic acid. The MS experiments were performed in selected ion monitoring mode (SIM). The method shows good linearity over the range of 0.1 - 5 mg/L for NA with a correlation coefficient of 0.9983. The limit of determination (LOD) was 0.05 mg/kg. Precision and recovery studies were evaluated at three concentration levels for rice root, stem, leaf and unpolished rice. The recovery (n = 5) ranged from 72.0% to 89.2% with relative standard deviations from 2.3% to 9.6%. The method is simple, highly selective and reliable, and can be Used to determine NA in rice at physiological level.

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