柱前衍生-高效液相色谱法测定食物和保健食品中维生素B_1  被引量:7

Determination of Vitamin B_1in Food and Health Food by High Performance Liquid Chromatography Coupled with Pre-column Derivatization

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作  者:华娟[1] 林光美[1] 傅武胜[2,3,4] 郑奎城[2,3,4] 吴少明 詹毓贤 

机构地区:[1]福建农林大学作物科学学院,福州350002 [2]福建省人兽共患病研究重点实验室福建省疾病预防控制中心,福州350001 [3]福建医科大学药学院,福州350108 [4]福建中医药大学,福州350122 [5]福建省产品质量检验研究院,福州350002

出  处:《中国食品学报》2014年第4期251-257,共7页Journal of Chinese Institute Of Food Science and Technology

基  金:卫生部2011年度食品安全国家标准立项计划项目(spaq-2011-47)

摘  要:目的:建立柱前衍生-高效液相色谱法(HPLC)测定食品中维生素B-含量的方法。方法:样品以0.1mol/L盐酸在120℃条件下高压提取,经2%碱性铁氰化钾溶液衍生后,以正丁醇液液萃取,用HPLC测定萃取物。采用SymmetryC18柱(150mm~4.6mm,5μm)分离,以0.05mol/L乙酸钠溶液-甲醇(体积比65:35)为流动相,荧光检测器检测(Ex=375nm,Em=435nm),外标法定量。结果:维生素B1在0.1~1.0mg/L范围内线性关系良好,相关系数大于0.9990;不同食品中维生素B1的检出限为0.2—0.3mg/kg,定量限为0.6—0.9mg/kg;对鸡蛋等4种食品基质进行加标试验,维生素B1的回收率均值为90.1%~109%,相对标准偏差(RSD)为1.9%-8.5%(n=6)。结论:该方法简单快速,灵敏度高,准确性好,可适用于各类食品和保健食品中维生素B1含量的测定。Objective:A simple method based on pre-column derivatization coupled with high performance liquid chromatography (HPLC) was developed for the determination of vitamin B1 in foods and health foods. Methods:The ho- mogenized food sample was extracted with 0.1 mol/L hydrochloric acid at 120℃ and the extract or the cleaned up solu- tion was derivatized with 2% alkaline potassium ferricyanide solution. The separation of the vitamin B1 deravatives extracted by butanol was achieved on a Symmetry C18 column (150 mm×4.6 mm,5μm)with 0.05 mol/L sodium acetate- methanol (65:35,V/V) as the mobile phase. The analyte was detected by the fluorescence detector (Ex--375 nm, Em=435 nm). The quantification was achieved by the external standard method. Results:Good linearity was observed in the range of 0.1-1.0 mg/L with the correlation coefficient 〉0.9990. The limits of detection and quantification for vitamin B1 were in the range of 0.2-0.3 mg/kg and 0.6-0.9 mg/kg for the selected foods, respectively. The average recoveries of vitamin B1 spiked in fresh egg, apple, potato and amcal were 90.1%-109% and the relative standard deviation (RSD) was 1.9%-8. 5%(n=6). Conclusion:Owing to the simplicity, rapidity, high sensitivity and accuracy, the method can be widely used for the quantification of vitamin B1 in the various foods and health foods.

关 键 词:食品 维生素B1 柱前衍生 高效液相色谱法 荧光检测器 

分 类 号:O657.72[理学—分析化学] TS207.3[理学—化学]

 

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