| 柱前衍生高效液相色谱-质谱法测定水稻中尼克烟酰胺含量 |
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| 引用本文： | 曹赵云,牟仁祥,陈铭学.柱前衍生高效液相色谱-质谱法测定水稻中尼克烟酰胺含量[J].分析化学,2009,37(7). |
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| 作者姓名： | 曹赵云 牟仁祥 陈铭学 |
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| 作者单位： | 中国水稻研究所,农业部稻米及制品质量监督检验测试中心,杭州,310006 |
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| 基金项目： | 国家自然科学基金，中央级公益性科研院所基本科研业务专项基金 |
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| 摘 要： | 建立了柱前衍生高效液相色谱-质谱联用(HPLC-MS)测定水稻中尼克烟酰胺含量的方法.样品中尼克烟酰胺经水提取后,与9-芴甲基氯甲酸酯(FMOC-Cl)衍生,采用液相色谱质谱联用仪测定.系统研究了衍生剂浓度和衍生介质等条件对衍生效率的影响.通过优化流动相酸度和梯度洗脱等条件,提高了方法灵敏度.尼克烟酰胺在0.1～5.0 mg/L范围内呈良好的线性关系(r=0.9983),对水稻的根、茎、叶及大米的标准加入实验表明,方法的添加回收率在72.0%～89.2%之间; 相对标准偏差为2.3%～9.6%; 方法检出限为0.05 mg/kg.方法简便、准确可靠,可以满足水稻中生理水平尼克烟酰胺的定性定量分析.
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| 关 键 词： | 尼克烟酰胺 水稻 柱前衍生 高效液相色谱 质谱 |
Determination of Nicotinamide in Rice by Pre-column Derivatization and High Performance Liquid Chromatography-Mass Spectrometry |
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| CAO Zhao-Yun,MOU Ren-Xiang,CHEN Ming-Xue.Determination of Nicotinamide in Rice by Pre-column Derivatization and High Performance Liquid Chromatography-Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2009,37(7). |
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| Authors: | CAO Zhao-Yun MOU Ren-Xiang CHEN Ming-Xue |
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| Institution: | CAO Zhao-Yun,MOU Ren-Xiang,CHEN Ming-Xue(Rice Product Quality Inspection and Supervision Center,Ministry of Agriculture,China National Rice Research Institute,Hangzhou 310006) |
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| Abstract: | 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-Cl).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 C18 column and... |
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| Keywords: | Nicotinamide rice prE-column derivatization liquid chromatography-mass spectrometry |
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