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分散液相微萃取和分散微固相萃取在高效液相色谱-二极管阵列检测法测定猪肌肉中喹诺酮类药物中的应用。

Application of dispersive liquid-liquid microextraction and dispersive micro-solid-phase extraction for the determination of quinolones in swine muscle by high-performance liquid chromatography with diode-array detection.

机构信息

Department of Food Science, National Pingtung University of Science & Technology, No. 1 Hseuh-Fu Road, Nei-Pu, 91201 Pingtung, Taiwan.

出版信息

Anal Chim Acta. 2009 Dec 10;656(1-2):56-62. doi: 10.1016/j.aca.2009.10.008. Epub 2009 Oct 9.

Abstract

Dispersive liquid-liquid microextraction (DLLME) and dispersive micro-solid-phase extraction (DMSPE) are two simple and low-cost sample preparation methods for liquid samples. In this work, these two methods were applied to solid tissue sample for the determination of seven quinolones by high-performance liquid chromatography with diode-array detection (HPLC-DAD). After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, small amounts of the extract were used for the DLLME and DMSPE methods. In the DLLME approach, the target analytes in the extraction solvent were rapidly extracted into a small volume of dichloromethane for drying and the residue was reconstituted for HPLC-DAD analysis. In the DMSPE approach, the target analytes in the extraction solvent were trapped by dispersive silica-based PSA (primary and secondary amine) sorbents and desorbed into a small amount of desorption solution for HPLC-DAD analysis. Under the optimal conditions, relative recoveries were determined for swine muscle spiked 50-200 microg kg(-1) and quantification was achieved by matrix-matched calibration. The calibration curves of seven quinolones showed linearity with a correlation coefficient value above 0.998 for both approaches. Relative recoveries ranged from 93.0 to 104.7% and from 95.5 to 111.0% for DLLME and DMSPE, respectively. Limits of detection (LODs) ranged from 5.6 to 23.8 microg kg(-1) and from 7.5 to 26.3 microg kg(-1) for DLLME and DMSPE, respectively.

摘要

分散液相微萃取 (DLLME) 和分散固相微萃取 (DMSPE) 是两种用于液体样品的简单、低成本的样品制备方法。在本工作中,将这两种方法应用于固体组织样品中,通过高效液相色谱-二极管阵列检测法 (HPLC-DAD) 测定七种喹诺酮类药物。在乙腈和盐促进分配的猪肌肉匀浆后,使用少量提取物进行 DLLME 和 DMSPE 方法。在 DLLME 方法中,萃取溶剂中的目标分析物迅速被萃取到少量二氯甲烷中进行干燥,残留物被重新溶解用于 HPLC-DAD 分析。在 DMSPE 方法中,萃取溶剂中的目标分析物被分散的基于硅胶的 PSA(伯胺和仲胺)吸附剂捕获,并解吸到少量的洗脱溶液中用于 HPLC-DAD 分析。在最佳条件下,对猪肌肉中添加的 50-200μgkg-1 的七种喹诺酮进行了相对回收率测定,并通过基质匹配校准进行了定量。两种方法的校准曲线均呈线性,相关系数值均大于 0.998。DLLME 和 DMSPE 的相对回收率分别为 93.0-104.7%和 95.5-111.0%。DLLME 和 DMSPE 的检测限 (LOD) 分别为 5.6-23.8μgkg-1 和 7.5-26.3μgkg-1。

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