鸡肌肉组织中四环素类和氟喹诺酮类药物多残留检测  

Determination of tetracyclines and fluoroquinolones multiresidue in chicken muscle by High-Liquid Chromatography

作　　者：郭黎明[1] 朱奎[1] 丁双阳[1,2] 江海洋[1,2] 李建成[1,2] 李晓薇[1,2] 

机构地区：[1]中国农业大学动物医学院,北京100193 [2]国家兽药残留基准实验室,北京100193

出　　处：《中国农业大学学报》2009年第5期98-102,共5页Journal of China Agricultural University

基　　金：国家"十一五"科技支撑项目资助(2006BAK02A09)

摘　　要：建立了能同时提取净化鸡肌肉组织中多残留的前处理并使用高效液相色谱分别检测的方法。样品经McIlvaine缓冲液、McIlvaine缓冲液-甲醇混合液提取后,过Oasis HLB固相萃取柱,5%甲醇(φ)淋洗,甲醇洗脱,40℃氮气吹干,磷酸-三乙胺缓冲液/乙腈复溶。样品四环素类药物用紫外检测器检测,波长365 nm,氟喹诺酮类药物用荧光检测器检测:激发波长280 nm,发射波长为480 nm。结果显示:鸡肌肉组织中4种四环素类药物OTC、TC的检测限是5μg/kg,CTC、DOXY的检测限是16μg/kg,回收率范围60.6%～89.1%,变异系数范围1.9%～14.3%;4种氟喹诺酮类药物的检测限均为2μg/kg,回收率范围77.5%～86.3%,变异系数范围2.8%～7.4%。说明该方法灵敏度高、适应性强,适用于鸡肌肉组织中上述4种四环素类药物和4种氟喹诺酮类药物残留的一次性检出。In this study, the multiresidue of oxytetracycline （OTC）, tetracycline （TC）, chlortetracycline （CTC）, doxytetracycline （DOXY）, ofloxacin （OFL）, norfloxacin （NOR）, ciprofloxacin （CIP） and enrofloxacin （ENR） were simultaneously extraction and purification from chicken muscle by HPLC. The homogenized samples were extracted with perchloric acid to remove proteins and the extracts were partitioned with Mcllvaine buffer and Mcllvaine-methanol buffer. Further cleanup was perfomed on Oasis HLB solid-phase column. The cartridge was washed with 5% methanol, eluted with methanol. The elution was vaporized to dryness with nitrogen at 40℃, and the dry residue was resolved in phosphoric acid-triethylamine-acetonitrile. Then the multriresidues were determined with UV detector at 365 nm and fluoroquinolones were determined by fluorescences detector with excitation at 280 nm, emission at 480 nm. Limits of detection （LOD） of OTC and TC were 5 ug/kg , CTC or DOXY were 16 ug/kg, the recoveries and the coefficient of variation （CV） of tetracyclines were 60.6% -89.1% and 1.9% - 14.3% respectively. LOD of fluoroquinolones were 2 ug/kg, while the recoveries and the coefficient of variation of fluoroquinolones were 77.5% - 86.3% and 2.8% - 7.4%, respectively. This method can be used for the sensitive and accurate determination of multiresidue in chicken muscle.

关 键 词：鸡肌肉 高效液相色谱 四环素类药物 氟喹诺酮类药物 多残留 

分 类 号：S851.4[农业科学—预防兽医学]