首页> 外文期刊>Journal of liquid chromatography and related technologies >Hollow fiber-based liquid phase microextraction coupled with high-performance liquid chromatography for extraction and determination of vitamin D3in biological fluids
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Hollow fiber-based liquid phase microextraction coupled with high-performance liquid chromatography for extraction and determination of vitamin D3in biological fluids

机译:中空纤维基液相微萃取结合高效液相色谱法用于生物液中维生素D3的提取和测定

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摘要

The reliability of hollow fiber-based on using two immiscible organic solvents in the lumen and wall pores of hollow fiber was evaluated for extraction and preconcentration of trace amount of vitamin D3, prior to determination by HPLC-UV. The analyte was extracted from a 8-mL sample solution, into a thin layer of an organic solvent (n-dodecane) impregnated in hollow fiber pores, and finally back-extracted into a μL volume of organic solvent (acetonitrile) located inside the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, hollow fiber length, stirring speed, extraction time, ionic strength, sample volume, and extraction temperature on the enrichment factors(EFs) were investigated. Under optimized conditions, the enrichment factor of 130, limit of detection (LOD) of 0.9ngmL-1 were obtained. The calibration curve was linear within the range of 3 to 1000ngmL-1 with reasonable linearity (R2=0.999). The percentages of relative within-day and between-day standard deviations (RSD %) based on six replicated determinations were 5.4 and 6.1, respectively. Finally, the feasibility of the proposed method was successfully evaluated by extraction, and determination of the analyte in the biological fluids and satisfactory results were obtained.
机译:在通过HPLC-UV测定之前,评估了中空纤维的可靠性,该方法基于在中空纤维的内腔和壁孔中使用两种不混溶的有机溶剂来提取和预富集痕量的维生素D3。将分析物从8毫升样品溶液中萃取到浸入空心纤维孔中的薄层有机溶剂(正十二烷)中,最后反萃取到位于内腔内部的微升体积的有机溶剂(乙腈)中中空纤维。研究了有机溶剂的性质,中空纤维长度,搅拌速度,萃取时间,离子强度,样品量和萃取温度等几个因素对富集因子(EFs)的影响。在优化的条件下,获得的富集因子为130,检测限(LOD)为0.9ngmL-1。校正曲线在3至1000ngmL-1范围内呈线性,并具有合理的线性(R2 = 0.999)。基于六次重复测定的日内和日间相对标准偏差(RSD%)的百分比分别为5.4和6.1。最后,通过萃取成功地评估了所提方法的可行性,并测定了生物液体中的分析物并获得了满意的结果。

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