固相萃取-二维液相色谱法同时测定婴儿配方乳粉中V_(A)、V_(D)和V_(E)  

Simultaneous determination of V_(A),V_(D)and V_(E)in infant formula milk powder by solid phase extraction with two-dimensional liquid chromatography

作　　者：宁霄[1] 金绍明[1] 刘彤彤 赵梅 曹进[1] NING Xiao;JIN Shaoming;LIU Tongtong;ZHAO Mei;CAO Jin(National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《化学分析计量》2023年第8期35-39,共5页Chemical Analysis And Meterage

摘　　要：建立了同时测定婴儿配方乳粉中V_(A)、V_(D)和V_(E)含量的固相萃取-二维液相色谱法。通过正交试验优化皂化条件,样品皂化液经TUP-E76-2060固相萃取柱净化后,以赛默飞FOODKIT1 ADE-C18色谱柱(150 mm×3.0 mm,3μm)作为一维分析柱,完成V_(A)和V_(E)的定量及V_(D)的净化,以赛默飞FOCDKIT1&2ADE-C18色谱柱(100 mm×4.6 mm,2.6μm)作为二维分析柱,完成对V_(D)的定量分析。结果显示,V_(A)、V_(D)和V_(E)分别在质量浓度为0.005~5、0.01~10和0.5~500μg/mL范围内与色谱峰面积具有良好的线性,相关系数分别为0.9996、0.9998和0.9999。与国标法比较,该方法在灵敏度、准确度及精密度等方面均有不同程度的提升,尤其是V_(A)的定量限提高了30倍,V_(D)的回收率提升了1.6倍。该方法样品处理过程简便快捷,准确稳健,可满足实验室大批量样品快速分析的需求。A new method for simultaneous determination of V_(A),V_(D)and V_(E)in infant formula milk powder by solid phase extraction(SPE)with two-dimensional liquid chromatography was developed.The saponification conditions were optimized by orthogonal experiment.Samples were cleaned up by TUP-E76-2060 SPE column after saponification.The quantifications of V_(A)and V_(E)and purification of V_(D)were completed simultaneously by the one-dimensional analysis with Thermo Field FOODKIT1 ADE-C18 column(150 mm×3.0 mm,3μm).A Thermo Feix FocdKIT1&2ADE-C18 column(100 mm×4.6 mm,2.6μm)was used as a two-dimensional column for the quantitative analysis of V_(D).The results showed that the mass concentration of V_(A),V_(D)and V_(E)had good correlation with the chromatogram peak area in the range from 0.005 to 5μg/mL,0.01 to 10μg/mL and 0.5 to 500μg/mL,respectively,and the correlation coefficients were 0.9996,0.9998 and 0.9999,respectively.Compared with the national standard method,the sensitivity,accuracy and precision of the method were improved to varying degrees.In particular,the limit of quantification of V_(A)was increased by 30 times,and the recovery of V_(D)was increased by 1.6 times.This method is simple of pretreatment process,fast,accurate and robust,which can meet the needs of rapid analysis of large quantities of samples in laboratory.

关 键 词：脂溶性维生素 婴儿配方乳粉 固相萃取 二维液相色谱 

分 类 号：O657[理学—分析化学]