聚合物整体柱管内固相微萃取-高效液相色谱在线联用测定血浆中的氟喹诺酮类药物

Determination of Five Fluoroquinolones in Human Plasma Using Polymer Monolith Microextraction Coupled to High-Performance Liquid Chromatography

目的建立一种聚（甲基丙烯酸-乙二醇二甲基丙烯酸酯）[P（MAA-co-EGDMA）]毛细管整体柱管内固相微萃取与高效液相色谱在线联用测定血浆中5种氟喹诺酮类药物的方法。方法本实验系统优化了5种氟喹诺酮类药物在P（MAA-co-EGDMA）整体柱上的萃取条件,选用25mmol·L^-1磷酸盐缓冲液（pH4.1）为固相微萃取携带液;解吸液及流动相均为25mmol·L^-1磷酸盐缓冲液（pH2.1）-甲醇-乙腈（72∶20∶8）;流速分别为0.04及1.0mL·min^-1;检测波长为280nm。结果建立的管内固相微萃取与高效液相色谱在线联用,在预处理和测定血浆中的5种氟喹诺酮类药物时,无基质干扰现象,线性关系r〉0.9995,日内、日间精密度RSD〈7%,检测限为1.1~2.6μg·L^-1。结论作为一种将样品的预处理及预富集与色谱分离检测在线联用的新方法,该方法对环境污染小,能够简便快速、准确及高灵敏度地检测血浆等生物样品中的药物含量。

OBJECTIVE To develop a method using in-tube solid phase microextraction （in-tube SPME） based on poly（MAA-co-EGDMA） monolith on-line coupled to HPLC with UV detection for the determination of five fluoroquinolones （FQs） in human plasma. METHODS The extraction conditions for five FQs on poly（MAA-co-EGDMA） monolith were optimized,25 mmol·L^-1 phosphate buffer was selected as the carrier buffer. 25 mmol·L^-1 phosphate buffer solution （pH 2.1）-acetonitrile-methanol （72 ： 8 ： 20） was selected as in-tube SPME desorption, and mobile phase, respectively. Their flow rates were at 0.04 mL·min^ -1 and 1.0 mL·min^ -1, respectively.The UV detection wavelength was set at 280 nm. RESULTS Under the optimized extraction conditions, good extraction efficiency for the five FQs was obtained with no matrix interference in the process of extraction and the following chromatographic separation. Good linearity （r〉0.999 5） and reproducibility （RSD〈7%） were achieved for the five FQs. The detection limits （S/N=3） of five FQs were found to be 1.1-2.6μg·L^-1 in plasma, respectively. CONCLUSION The high extraction efficiency of the in-tube SPME based on poly（MAA-co-EGDMA） monolithic for zwitterionic FQs from plasma samples was demonstrated. In comparison to existing sample pretreatment methods for FQs in plasmas, a simpler, more rapid and sensitive in-tube SPME method was demonstrated.