建立了同时检测动物肌肉组织中9种喹诺酮类药物、7种磺胺类药物和甲氧苄啶的高效液相色谱检测方法。动物肌肉组织样品用磷酸盐缓冲液提取,HLB固相萃取柱净化,洗脱液用氮气吹至近干,磷酸盐缓冲液复溶,以甲酸水溶液-乙腈体系为流动相,梯度洗脱,荧光-紫外检测器串联测定。本方法的线性良好,相关系数r〉0.9987;平均回收率为70.6%~103.4%,相对标准偏差为1.2%~11.4%;荧光检测器测定喹诺酮类药物的检出限为0.04~0.4μg/kg;紫外检测器测定磺胺类药物和甲氧苄啶的检出限为3.5μg/kg。本方法具有简便、通用性强的特点,适用于动物肌肉组织中上述药物的常规残留检测。
A multiresidue analytical method was developed for the determination of 9 quinolones( marbofloxatin, ofloxacin, lomefloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, oxolinic acid and flumequine) , 7 sulfonamides( sulfadiazine, sulfapyridine, sulfathiazole, sulfadimidine, sulfamonomethoxine, sulfamethoxazole and sulfahenzamide) , and trimethoprim in swine and chicken muscle tissues by high performance liquid chromatography. The samples were extracted with phosphate buffer solution and cleaned up with a hydrophilic-lipophilic balance solid-phase extraction cartridge. The collected eluent was evaporated to near dryness under a nitrogen stream and reconstituted in phosphate buffer solution. The analytes were separated using formic acid aqueous solution-acetontrile system as mobile phase with a linear gradient elution program, and determined by ultraviolet detection tandem programmable fluorescence detection. Linear of the method was fine with correlation coefficients(r) more than 0. 9987. The mean recoveries for each drug in swine and chicken muscles ranged from 70.6% to 103.4% with relative standard deviation below 11.4%. The limit of quantification was 0.2 - 2.0 μg/kg for quinolones, and 12μg/kg for sulfonamides and trimethoprim. The limit of detection was 0.04 - 0.4μg/kg for quinolones, and 3.5 μg/kg for sulfonamides and trimethoprim. This simple and sensitive method can be used to determine the residues of these drugs in actual samples.