分散液液微萃取-高效液相色谱联用测定水样中的氟喹诺酮类药物

建立了一种分散液液微萃取-高效液相色谱联用测定水样中6种氟喹诺酮类药物的方法,采用萃取剂萃取后经氮气吹干再用微量流动相复溶的进样方式,考察了影响萃取效率的因素,包括萃取剂和分散剂的种类、用量、样品pH。结果表明,以500μL三氯甲烷为萃取剂,800μL乙腈为分散剂,调节萃取体系pH为7时,6种氟喹诺酮药物的富集倍数最高可达245倍,检出限为0.075⁰.34μg/L。在汉江水、鱼塘水、自来水中的加标回收率为88.6%¹09.3%,相对标准偏差不高于5.8%。该方法基质效应小,富集倍数高,并且改善了传统DLLME萃取后的萃取剂直接进样色谱峰变形的缺点。应用于水样中残留氟喹诺酮类药物的检测,灵敏度高、简便、准确。 

Determination of fluoroquinolones in water with dispersive liquid-liquid phase microextraction-HPLC

Dispersive liquid-liquid micro-extraction coupled with high performance liquid chromatography ( DLLME-HPLC) was applied to separate and determine six fluoroquinolones ( FQs) in aqueous samples.Before injection into HPLC, the extraction solvent droplet obtained after centrifugation was pulled out, and then dried by nitrogen flow, re-dissolved with dozens of microliters mobile phase at last.Some important parameters, like variety and dosage of extractant and dispersive solvent and pH of extraction solution, which influent the extraction efficiency were investigated. The results showed that after adding 500 μL trichloromethane as extractant solvent, 800 μL acetonitrile as dispersive solvent into extraction system which p H was tuned to7, enrichment factor of 6 FQs was up to 245 and a good linear relationship was obtained in the range of 0.075~0.34 μg/L.The recoveries of 6 FQs in 3 kinds of water from han river, fishpond and running water fell in the range from 88.6% to 109.3% and the relative standard deviation was less than 5.8%. The method had low matrix effect, high enrichment factor and avoids chromatographic peak deformation when direct injection of extraction solvent droplet in the traditional DLLME.It was proven to be sensitive, simple, and accurate in residue analysis of FQs in water.