高效液相色谱荧光检测器测定氟喹诺酮类药物残留方法的建立  

A Method for Determination of Fluoroquinolone Residues by HPLC with Fluorescence Detector

作　　者：杨勇[1,2] 罗奕[3] 苏菊[3] 吴琳琳[3] 茅向军[2] 许乾丽[2] 

机构地区：[1]贵阳中医学院,贵阳550002 [2]贵州省食品药品检验所,贵阳550004 [3]贵州医科大学,贵阳550004

出　　处：《中国农业科技导报》2016年第2期176-181,共6页Journal of Agricultural Science and Technology

基　　金：贵州省食品;保健食品和化妆品监测检测平台项目(黔科平台[2012]4001);贵州动物源性食品氟喹诺酮类药残留检测及快速筛查技术研究项目(黔科合SY字[2012]3061号)资助

摘　　要：为了探索经济适用的氟喹诺酮类残留提取和检测方法,建立了同时测定牛奶中6种氟喹诺酮类药物残留的高效液相色谱（HPLC）串联荧光检测器（FLD）检测方法。样品经过含有5%乙酸的乙腈溶液涡旋提取,经改良Qu ECh ERS方法净化,HPLC-FLD检测,激发波长280 nm,发射波长450 nm,色谱柱为Waters XBridgeTM-C18柱（4.6 mm×250 mm,5μm）,流速1.0 m L/min,柱温30℃,以乙腈和含0.1%甲酸的20 mmol/L甲酸铵水溶液做为流动相进行梯度洗脱。在所建立的方法中6种氟喹诺酮分离度较好（R〉1.5）,在0.01~0.3μg/m L浓度范围内具有良好的关系（r=0.999 9）,检出限在0.97~3.91μg/kg之间,回收率试验中平均加标回收率为97%~100%;重复性、精密度、稳定性试验结果良好,相对标准偏差均〈3%。所建立方法简单、快速、灵敏度和回收率高,适用于牛奶中该6种氟喹诺酮类药物残留的大批量筛选和定量测定。In order to develop a high performance liquid chromatography,high performance liquid chromatography series fluorescence detector（ HPLC-FLD） detection method was established,which could detected 6 fluoroquinolones residues in milk at the same time. The sample after acetonitrile containing 5% acetic acid extraction of the vortex,the modified Qu ECh ERS method of HPLC-FLD purification,detection,excitation wavelength 280 nm and emission wavelength of 450 nm,the column was Waters XBridge TM-C18column（ 4.6 mm×250 mm,5 μm）,the flow rate of 1m L / min,the column temperature of 30℃,with acetonitrile and 0. 1% formic acid. 20 mmol / L ammonium formate solution as mobile phase gradient elution. In the method of good separation of 6 fluoroquinolones（ R1.5）,in 0.01 ~0.3 g / m L concentration range with good relationship（ r = 0.999 9）,the detection limit is between 0.97 ~ 3.91 g / kg,the recovery rate of test in the average recovery rate was 97% ~ 100%. Repeatability,precision,stability test results are good,the relative standard deviation are 3%. The established method is simple,rapid,sensitive and high recovery rate,suitable for mass screening and quantitative determination of 6 kinds of fluoroquinolones residue in milk.

关 键 词：HPLC-FLD 牛奶 氟喹诺酮类 药物残留 

分 类 号：S859.84[农业科学—临床兽医学] TS207.5[农业科学—兽医学]