León-González M E, Rosales-Conrado N
Analytical Chemistry Department, Faculty of Chemistry, Complutense University of Madrid, E-28040 Madrid, Spain.
Analytical Chemistry Department, Faculty of Chemistry, Complutense University of Madrid, E-28040 Madrid, Spain.
J Chromatogr A. 2017 Sep 8;1514:88-94. doi: 10.1016/j.chroma.2017.07.072. Epub 2017 Jul 25.
A mixture of β-cyclodextrin (β-CD) and primary and secondary amine (PSA) sorbents was employed for the extraction and quantification of ibuprofen enantiomers from human breast milk, combining a vortex-assisted matrix solid-phase dispersion method (MSPD) and direct chiral liquid chromatography (CLC) with ultraviolet detection (UV). The MSPD sample preparation procedure was optimized focusing on both the type and amount of dispersion/sorption sorbents and the nature of the elution solvent, in order to obtain acceptable recoveries and avoiding enantiomer conversion. These MSPD parameters were optimized with the aid of an experimental design approach. Hence, a factorial design was used for identification of the main variables affecting the extraction process of ibuprofen enantiomers. Under optimum selected conditions, MSPD combined with direct CLC-UV was successfully applied for ibuprofen enantiomeric determination in breast milk at enantiomer levels between 0.15 and 6.0μgg. The proposed analytical method also provided good repeatability, with relative standard deviations of 6.4% and 8.3% for the intra-day and inter-day precision, respectively.
采用β-环糊精（β-CD）与伯胺和仲胺（PSA）吸附剂的混合物，结合涡旋辅助基质固相分散法（MSPD）和直接手性液相色谱法（CLC）及紫外检测（UV），从人母乳中提取和定量布洛芬对映体。以分散/吸附吸附剂的类型和用量以及洗脱溶剂的性质为重点，对MSPD样品制备程序进行了优化，以获得可接受的回收率并避免对映体转化。借助实验设计方法对这些MSPD参数进行了优化。因此，采用析因设计来识别影响布洛芬对映体提取过程的主要变量。在选定的最佳条件下，MSPD与直接CLC-UV联用成功用于测定母乳中对映体水平在0.15至6.0μg/g之间的布洛芬对映体。所提出的分析方法还具有良好的重复性，日内精密度和日间精密度的相对标准偏差分别为6.4%和8.3%。
