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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 establish a method for the determination of 5 kinds of poly (methacrylic acid-ethylene glycol dimethacrylate) [P (MAA-co-EGDMA)] capillary column solid phase microextraction and high performance liquid chromatography Fluoroquinolones. Methods The extraction conditions of five fluoroquinolones on P (MAA-co-EGDMA) monolithic column were optimized. 25mmol·L-1 phosphate buffer (pH4.1) was used as solid phase microextraction carrier ; The desorption solution and mobile phase were 25 mmol·L-1 phosphate buffer (pH 2.1) -methanol-acetonitrile (72:20:8); the flow rates were 0.04 and 1.0 mL · min-1 respectively; the detection wavelength was 280 nm . Results The in-tube solid-phase microextraction coupled with high performance liquid chromatography (HPLC) showed no matrix interference in the pretreatment and determination of five fluoroquinolones in plasma. The linear relationship was r> 0.9995. The intra- and inter-day precision RSD <7%, the detection limit of 1.1 ~ 2.6μg · L-1. Conclusion As a new method for on-line sample pretreatment and pre-enrichment and chromatographic separation, this method is simple, rapid, accurate and sensitive to detect drug content in biological samples such as plasma.