HPLC-FLD同时测定大米中8种维生素E  

Simultaneous Determination of 8 Kinds of Vitamin E in Rice by HPLC-FLD

作　　者：赵海燕[1] 李兵[1] 柳静 赵榕[1] 罗仁才[1] ZHAO Haiyan;LI Bing;LIU Jing;ZHAO Rong;LUO Rencai(Beijing Center for Disease Control and Prevention,Beijing 100013,China.)

机构地区：[1]北京市疾病预防控制中心,北京100013

出　　处：《预防医学情报杂志》2021年第8期1154-1158,1163,共6页Journal of Preventive Medicine Information

摘　　要：目的建立HPLC-FLD测定食用大米中8种维生素E(α、β、γ、δ生育酚和α、β、γ、δ三烯生育酚)的方法。方法食用大米直接用乙醇/二甲亚砜(15/5)超声提取离心后,取上清液测定。实验采用Dikma Inspire PFP(5μm,250×4.6 mm)色谱柱,以甲醇/水作为流动相梯度洗脱,使用FLD检测器检测(λex=296 nm,λem=325 nm)。结果方法的线性范围:δ生育酚0.0488~4.88μg/ml、β生育酚0.0387~3.87μg/ml、γ生育酚0.0528~5.28μg/ml、α生育酚0.0553~5.53μg/ml和δ三烯生育酚0.0472~4.72μg/ml、β三烯生育酚0.0484~4.84μg/ml、γ三烯生育酚0.0445~4.45μg/ml、α三烯生育酚0.044~4.40μg/ml,相关系数R均大于0.9997。方法定性检出限(s/n=3)δ三烯生育酚、β三烯生育酚、γ三烯生育酚、α三烯生育酚、δ生育酚、β生育酚、γ生育酚和α生育酚分别为:0.0213、0.0255、0.0261、0.0198、0.0216、0.0180、0.0252和0.0306μg/g;定量检出限(s/n=10):0.071、0.085、0.087、0.066、0.072、0.060、0.084和0.102μg/g;8种组分按高、中、低3个浓度水平加标,平均回收率为94%~104.9%,相对标准偏差RSD(n=6)均<3%。结论本方法简便稳定,准确灵敏,适用于食用大米中8种维生素E的同时测定。Objective To establish an High Performance Liquid Chromatography(UPLC)with Fluorescence Detector(FLD)method for determination of 8 kinds of vitamin E(α、β、γ、δ-tocopherol andα、β、γ、δ-trientocopherol)in edible rice.Methods The rice samples were extracted ultrasonically centrifugation with dimethyl sulfoxide-ethanol(5∶15),and the supernatant was determined.The separation of compounds was carried out on an Dikma Inspire PFP column(5μm,250×4.6 mm)by gradient elution with methanol and water system.FLD detector was used,the fluorescence detection was performed with the excitation at 296 nm and the emission at 325 nm.Results The linearity ranges were 0.0488-4.88μg/ml forδ-tocopherol,0.0387-3.87μg/ml forβ-tocopherol,0.0528-5.28μg/ml forγ-tocopherol,0.0553-5.53μg/ml forα-tocopherol,0.0472-4.72μg/ml forδ-trientocopherol、0.0484-4.84μg/ml forβ-trientocopherol、0.0445-4.45μg/ml forγ-trientocopherol、and 0.044-4.40μg/ml forα-trientocopherol.The correlation coefficients R were not less than 0.9997.The limits of detection(s/n=3)of 8 vitamin E were 0.0213,0.0255,0.0261,0.0198、0.0216、0.0180、0.0252、0.0306μg/g,and the limits of quantitation(s/n=10)were 0.071、0.085、0.087、0.066、0.072、0.060、0.084、0.102μg/g(δ-、β-、γ-、α-trientocopherol、δ-、β-、γ-、α-tocopherol in turn).The mean recoveries ranged from 94%-104.9%at different spiked levels with relative standard deviations(RSD)were less than 3%.Conclusion The method is simple,stable,accurate and sensitive,and it is suitable for the simultaneous determination of 8 kinds of vitamin E in edible rice.

关 键 词：维生素E 生育酚 三烯生育酚 大米 HPLC 

分 类 号：R155[医药卫生—营养与食品卫生学]