CAJ | 학술논문

采用固相萃取与双梯度高效液相色谱联用技术,建立了一种在线固相萃取-高效液相色谱同时测定动物源食品中维生素A、E的分析方法。样品于80℃下皂化反应30 min,经离心沉淀后引入一维C8固相萃取柱,采用60%( V/V)甲醇溶液对目标物进行在线富集净化,然后通过阀切换将其转移至二维液相分析系统进行分离检测。考察了萃取填料、上样溶剂及洗脱条件对猪肝、鸡蛋和配方乳粉的维生素A、E富集和基质净化效果。结果表明,在优化条件下,方法线性范围为0.02~20 mg/L,线性相关系数R2≥0.9998,对维生素A、E的检出限(S/N=3)为3.0~30.0μg/L,实际样品加标回收率为87.3%~115.0%,相对标准偏差(RSD)为1.8%~4.6%。本方法操作简便,灵敏度高,可用于动物源食品中维生素A、E的快速测定。
채용고상췌취여쌍제도고효액상색보련용기술,건립료일충재선고상췌취-고효액상색보동시측정동물원식품중유생소A、E적분석방법。양품우80℃하조화반응30 min,경리심침정후인입일유C8고상췌취주,채용60%( V/V)갑순용액대목표물진행재선부집정화,연후통과벌절환장기전이지이유액상분석계통진행분리검측。고찰료췌취전료、상양용제급세탈조건대저간、계단화배방유분적유생소A、E부집화기질정화효과。결과표명,재우화조건하,방법선성범위위0.02~20 mg/L,선성상관계수R2≥0.9998,대유생소A、E적검출한(S/N=3)위3.0~30.0μg/L,실제양품가표회수솔위87.3%~115.0%,상대표준편차(RSD)위1.8%~4.6%。본방법조작간편,령민도고,가용우동물원식품중유생소A、E적쾌속측정。
An automated analytical method for simultaneous determination of vitamin A and E in livers, fortified infant formulae and eggs has been developed based on on-line solid phase extraction (SPE) coupled with a dual gradient high performance liquid chromatography system with column-switching. Firstly, food samples were centrifuged after saponified in mixture solution of anhydrous alcohol, potassium hydroxide and ascorbic acid at 80 ℃ for 30 min. Secondly, the saponified sample was loaded and washed on the first dimension extraction column using methanol-water (60∶40, V/V). Afterwards, the targeted analytes were trapped and enriched on the SPE column. Finally, the trapped analytes were transferred to the second dimension analysis column by valve-switching technique for the following separation and determination. Several key factors such as the type of SPE columns, elution buffer as well as pH of washing solution were optimized. The results showed that the calibration curves of vitamin A and E were linear in the range of 0 . 02-20 mg/L with correlation coefficient (R2) more than 0. 9998. In addition, the limits of detection (S/N=3) were found in the range of 3. 0-30. 0 μg/L. The spiked recoveries of the vitamin A and E from livers, eggs and fortified infant formulae ranged from 87 . 3% to 115 . 0% with the relative standard deviations ( RSDs ) of 1 . 8% -4 . 6%. The developed method is simple, sensitive and rapid to determine vitamins A and E in animal derived food.