柱切换法液相色谱测定保健食品中的VA、VD、VE  

Determination of Vitamins A,D and E in Health Foods Using Column-Switching Liquid Chromatography

作　　者：张丽媛 戚绿叶 周明昊 ZHANG Liyuan;QI Lüye;ZHOU Minghao(Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)

机构地区：[1]浙江省食品药品检验研究院,浙江杭州310052

出　　处：《食品科学》2022年第4期225-230,共6页Food Science

基　　金：浙江省健康产品化妆品行业协会团体标准项目(T/ZHCA-YSP2019001)。

摘　　要：建立柱切换法液相色谱测定保健食品中VA、VD、VE含量的方法。参照GB 5009.82—2016《食品中维生素A、D、E的测定》样品前处理方法,以Agilent Poroshell 120 PFP(4.6 mm×100 mm,2.7μm)为一维色谱柱,甲醇、水为流动相梯度洗脱,分离VA和VE的4种异构体,以Agilent Zorbax Eclipse PAH(2.1 mm×100 mm,3.5μm)为二维色谱柱,甲醇、乙腈为流动相梯度洗脱,分离VD_(2)和VD_(3)。以Agilent Poroshell 120 EC C_(18)(4.6 mm×5 mm,4μm)为捕获柱,捕获VD。根据VD在一维色谱柱上的出峰起止时间,确定柱切换时间。一维检测波长为325 nm和294 nm,二维检测波长为264 nm。以外标定量法测定VA、VD、VE的含量。结果表明,VA在2.50~50.0μg/mL、VD在0.10~2.00μg/mL、VE在5.00~100.0μg/mL线性范围内线性良好,相关系数均大于0.999。回收率为86%~102%,相对标准偏差为1.5%~4.0%。表明该方法测定准确,适用于保健食品中VA、VD、VE的含量测定。A method for the determination of vitamins A(VA),D(VD)and E(VE)in health foods by column-switching two-dimensional liquid chromatography was established.According to the sample pretreatment method specified in the national standard GB 5009.82-2016,VA and four isomers of VE were separated on an Agilent Poroshell 120 PFP column(4.6 mm×100 mm,2.7μm)as one-dimensional chromatographic column using a mobile phase consisting of methanol and water by gradient elution,and VD_(2) and VD_(3) were separated on an Agilent Zorbax Eclipse PAH column(2.1 mm×100 mm,3.5μm)by gradient elution using a mobile phase composed of methanol and acetonitrile.VD was captured on an Agilent Poroshell 120 EC C_(18) column(4.6 mm×5 mm,4μm).According to the peak time of VD on the one-dimensional chromatographic column,the column switching time was determined.The one-dimensional detection wavelengths were 325 and 294 nm,and the two-dimensional detection wavelength was 264 nm.The analytes were quantified by external standard method.Results indicated that the calibration curves were linear in the range of 2.50-50.0μg/mL for VA,and 0.10-2.00μg/mL for VD,and 5.00-100.0μg/mL for VE,and the correlation coefficients were all more than 0.999.The recoveries were 86%–102%,with relative standard deviations(RSD)of 1.5%–4.0%.The results suggest that the developed method is accurate and suitable for the determination of VA,VD and VE in health foods.

关 键 词：二维液相色谱 VA VD VE 保健食品 

分 类 号：TS207.3[轻工技术与工程—食品科学]