摘要
文章建立了在线固相萃取-二维高效液相色谱法测定婴幼儿配方乳粉中V_(A)、V_(D2)、V_(D3)和α-生育酚、β-生育酚、γ-生育酚、δ-生育酚的方法。样品经皂化处理后上机,固相萃取柱在线净化,一维色谱柱为Agilent Poroshell 120 PFP,流动相甲醇、水梯度洗脱,完成V_(A)和V_(E)异构体的分离定量及V_(D)的净化。以Agilent Poroshell 120 EC C_(18)为捕获柱,通过中心切割阀切换将V_(D)馏分转移至二维色谱系统。Agilent Zorbax Eclipse PAH为二维色谱柱,流动相甲醇、乙腈梯度洗脱,实现V_(D2)和V_(D3)分离及定量。一维可变波长紫外检测器波长为325 nm和294 nm,二维二极管阵列检测器波长为264 nm。外标法定量。在最优仪器条件下,V_(A)、V_(D2)、V_(D3)和4种V_(E)同分异构体线性关系良好,相关系数均大于0.9996,方法回收率为90.2%~98.6%,相对标准偏差为0.17%~0.94%。该方法简单、快速、准确,适用于婴幼儿配方乳粉中V_(A)、V_(D)、V_(E)的测定,可为企业内部质量控制和监管部门快速应急处置食品安全风险突发事件提供技术保障。
To establish an online solid phase extraction system and two-dimensional liquid chromatography method for the determination of V_(A),V_(D2),V_(D3),α-tocopherol,β-tocopherol,γ-tocopherol andδ-tocopherol in infant formula.Samples after saponification treatment on the machine,solid phase extraction column online purification,Agilent Poroshell 120 PFP is a one-dimensional column,gradient elution of methanol and water was used as flow phase,separation and quantification of V_(A) and four isomers of V_(E) and purification of V_(D).Using Agilent Poroshell 120 EC C_(18) as the capture column,the V_(D) fraction was transferred to the two-dimensional chromatography system by switching the central cutting valve.Agilent Zorbax Eclipse PAH was a two-dimensional column,methanol and acetonitrile were used for gradient elution,V_(D2) and V_(D3) were isolated and quantified,the detection wavelength of one-dimensional VWD detector was 325 nm and 294 nm,and the detection wavelength of two-dimensional DAD detector was 264 nm.Quantification by external standard method.Under optimal instrument conditions,V_(A),V_(D2),V_(D3)and four kinds of VE isomers showed good linear relationship in their respective linear range,the correlation coefficients were all more than 0.9996,the recoveries were 90.2%~98.6%,the relative standard deviations were 0.17%~0.94%.The method is simple,rapid and accurate,which is suitable for the determination of V_(A),V_(D)and vitamin E in infant formula milk powder,and can provide technical support for the internal quality control of enterprises and the supervision department to deal with food safety risk emergencies quickly.
作者
安永鹏
宋杰
林立
丁轲
高杨
AN Yongpeng;SONG Jie;LIN Li;DING Ke;GAO Yang(Beijing Municipal Center for Food Safety Monitoring and Risk Assessment,Beijing 100094,China;Department of Food Science and Engineering,Beijing University of Agriculture,Beijing 102206,China)
出处
《食品科技》
CAS
北大核心
2022年第7期261-267,共7页
Food Science and Technology
基金
国家重点研发计划项目(2017YFC1601003)
北京市自然科学基金项目(KZ201710020014)。
