Determination of <italic style="font-style: italic">Cis</italic> and <italic style="font-style: italic">Trans</italic> Isomers of Retinol and <italic style="font-style: italic">α</italic>-Tocopherol Chiral Isomers in Infant Formula by Online Solid Phase Extraction and Two-dimensional Liquid Chromatography

TIE Xiao-wei; XIE Min; HUANG Bai-fen; SHI Hong-bo; REN Yi-ping

doi:10.19969/j.fxcsxb.23042401

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Determination of Cis and Trans Isomers of Retinol and α-Tocopherol Chiral Isomers in Infant Formula by Online Solid Phase Extraction and Two-dimensional Liquid Chromatography

Experimental Techniques and Methods | 更新时间：2023-09-19

- Determination of Cis and Trans Isomers of Retinol and α-Tocopherol Chiral Isomers in Infant Formula by Online Solid Phase Extraction and Two-dimensional Liquid Chromatography
- Journal of Instrumental Analysis Vol. 42, Issue 9, Pages: 1174-1180(2023)
- 作者机构：
  
  1.欧陆分析技术服务（苏州）有限公司，江苏苏州 215163
  2.浙江省疾病预防控制中心，浙江杭州 310057
  3.浙江大学生物系统工程与食品科学学院，浙江杭州 310058
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23042401
  CLC：
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铁晓威,谢敏,黄百芬等.在线固相萃取/二维液相色谱法检测婴幼儿配方食品中视黄醇顺反异构体和α-生育酚手性异构体[J].分析测试学报,2023,42(09):1174-1180.

TIE Xiao-wei,XIE Min,HUANG Bai-fen,et al.Determination of Cis and Trans Isomers of Retinol and α-Tocopherol Chiral Isomers in Infant Formula by Online Solid Phase Extraction and Two-dimensional Liquid Chromatography[J].Journal of Instrumental Analysis,2023,42(09):1174-1180.
铁晓威,谢敏,黄百芬等.在线固相萃取/二维液相色谱法检测婴幼儿配方食品中视黄醇顺反异构体和α-生育酚手性异构体[J].分析测试学报,2023,42(09):1174-1180. DOI： 10.19969/j.fxcsxb.23042401.

TIE Xiao-wei,XIE Min,HUANG Bai-fen,et al.Determination of Cis and Trans Isomers of Retinol and α-Tocopherol Chiral Isomers in Infant Formula by Online Solid Phase Extraction and Two-dimensional Liquid Chromatography[J].Journal of Instrumental Analysis,2023,42(09):1174-1180. DOI： 10.19969/j.fxcsxb.23042401.

摘要

建立了在线固相萃取/二维液相色谱分离检测婴幼儿配方食品中全反式视黄醇、13-顺式视黄醇和,α,-生育酚手性异构体的方法。样品经皂化，定容、离心、过滤后进样，经二乙烯基苯与N-乙烯基吡咯烷酮大孔共聚物（HLB）在线固相萃取柱在线净化后，通过切换阀将视黄醇、4种生育酚洗脱至一维色谱柱五氟苯基填料柱（PFP），在一维色谱柱中实现总视黄醇和4种生育酚异构体的分离。再通过捕集柱与中心切换阀将总视黄醇和,α,-生育酚切割至二维色谱柱，在3，5-二甲基苯基氨基甲酸酯涂敷的手性色谱柱（CND）上实现了全反式与13-顺式视黄醇的异构体分离，以及,α,-生育酚的,d,、,l,手性异构体分离。采用紫外和荧光检测器检测，外标法定量。结果表明：全反式视黄醇、13-顺式视黄醇的线性范围为0.1~5.0 mg/L，,d,-,α,-生育酚、,l,-α-生育酚的线性范围为1.0 ~ 30.0 mg/L，相关系数均大于0.999，定量下限分别为53 μg/100 g、56 μg/100 g、290 μg/100 g和340 μg/100 g；低、中和高3个加标浓度下的回收率为90.9% ~ 106%，相对标准偏差（RSD）不大于2.8%。该方法可用于乳基婴幼儿配方食品中视黄醇和,α,-生育酚的检测及其生物有效性评价。

Abstract

A quantitative determination method for the separation of all-,trans, retinol，13-,cis,-retinol and ,α,-tocopherol chiral isomers in infant formula was established by online solid phase extraction and two-dimensional liquid chromatography technique. After sample was purified by divinylbenzene and N-vinylpyrrolidone macroporous copolymer（HLB） online solid phase extraction column，retinol and four tocopherols were eluted to the first-dimensional high performance liquid chromatography with pentafluorophenyl packing column（PFP） by switching valve，and the total retinol and four tocopherol isomers were separated in the first-dimensional column. The total retinol and ,α,-tocopherol were cut sequentially into the second-dimensional column by the trap column and the central switching valve，then the separation of all-,trans, and 13-,cis,-retinol isomers was realized in the chiral column（CND） coated with 3，5-dimethylphenylcarbamate，and the separation of ,d, and ,l, chiral isomers of ,α,-tocopherol was realized at the same time. All of the compounds are detected by ultraviolet and fluorescent detectors with external standard quantification. The linear range was 0.1-5.0 mg/L for all-,trans, retinol and 13-,cis,-retinol，1.0-30.0 mg/L for ,d,- and ,l,-,α,-tocopherol with correlation coefficients more than 0.999，and the quantitation limits of all-,trans, retinol，13-,cis,-retinol，,d,- and ,l,-,α,-tocopherol were 53 μg/100 g，56 μg/100 g，290 μg/100 g，and 340 μg/100 g respectively. Recoveries at low，medium and high spiked concentrations were between 90.9%-106%，with relative standard deviations（RSD） not more than 2.8%. The method could meet the regular analysis of retinol and ,α,-tocopherols in milk-based infant formula，and also the exact evaluation of their bioavailability after considering relative bioactive factor for each.

关键词

HLB在线固相萃取CND涂敷手性分离柱视黄醇顺反异构体α-生育酚手性异构体婴幼儿配方食品

Keywords

HLB online solid phase extractionCND-coated chiral separation columncis and trans-retinol isomersα-tocopherol chiral isomersinfant formula

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Determination of Cis and Trans Isomers of Retinol and α-Tocopherol Chiral Isomers in Infant Formula by Online Solid Phase Extraction and Two-dimensional Liquid Chromatography

DOI：10.19969/j.fxcsxb.23042401

摘要

Abstract

关键词

Keywords

references