超高效液相色谱法同时测定鸡肝中五种氟喹诺酮类药物残留

Simultaneous analysis of five fluoroquinolones residues in chicken liver by Ultra Performance Liquid Chromatography

关键词:  超高效液相色谱  固相萃取  氟喹诺酮类药物  多残留检测  鸡肝

Key words:  Ultra Performance Liquid Chromatography (UPLC)  Solid phase extraction (SPE)  Fluoroquinolones  Simultaneous determination  chicken liver

摘要:

建立了一种同时测定鸡肝中五种氟喹诺酮类药物残留的超高效液相色谱检测法（UPLC）。样品经磷酸盐缓冲溶液提取、C18柱净化，采用ACQUITY UPLCTM BEH C18色谱柱（50×2.1mm，1.7μm）分离，以乙腈溶液和0.1%甲酸的水溶液作为流动相进行等度洗脱，荧光检测器检测。五种药物在0.005~0.5μg/ml范围内线性关系良好，相关系数（r）均大于0.999；以0.05、0.15、0.30μg/g三个浓度水平进行添加回收试验，平均回收率都在70.2%~98.2%之间，相对标准偏差为4.6%~12.1%，方法的检出限（LOD）为0.02μg/g，定量限（LOQ）为0.05μg/g。方法重现性好、灵敏度高、简单、快捷，适用于鸡肝中五种氟喹诺酮类药物多残留的检测。

Abstract:

A method of ultra performance liquid chromatography (UPLC) for the simultaneous determination of five fluoroquinolones residues in chicken liver was developed. The sample was extracted with phosphate solution, purified by C18 pole, The UPLC separation was performed on an ACQUITY UPLCTM BEH C18 column(50×2.1mm，1.7μm) utilizing a equal elution program of acetonitrile and water (containing 0.1% formic acid) as the mobile phase. The linear ranges were from 0.005 to 0.5μg/ml with the relative standard deviations of coefficients above 0.999 for all five fluoroquinolones. The average recoveries spiked at the 3 concentration levels of 0.05、0.15、0.30μg/g ranged from 70.2% to 98.2% with the relative standard deviations of 4.6% to 12.1%. The limits of detection （LOD）were 0.02μg/g and the limits of quantitation（LOQ） were 0.05μg/g. The method was proved to be good reproducibility, high sensitivity, simple, rapid and suitable for the simultaneous determination of multi-residues of fluoroquinolones in chicken liver.