猪组织中硫酸头孢喹肟含量测定和肌注给药残留研究

Detemination cefquinome sulphate in swine tissues and residues after intramuscular injection

建立了硫酸头孢喹肟在仔猪组织内残留的高效液相色谱分析法.色谱条件：采用C18色谱柱（4.6 mm×150 mm,5μm）,称取一水合高氯酸钠3.45 g溶于1 000 mL水中,加磷酸12 mL,用三乙胺调至pH3.6,将此溶液与乙腈按90∶10的比例混合作为流动相,紫外检测波长为270 nm.将头孢喹肟以20、100、500μg/kg分别添加到空白组织中,测得肌肉、肝脏、肾脏、肺脏、脂肪＋皮肤组织中头孢喹肟回收率均在78%以上,平均回收率分别为81.57%、82.42%8、1.29%8、3.97%、78.80%.日内变异RSD在1.82%~6.25%之间,日间变异RSD在1.11%~6.35%之间.该方法的最低检测限为20μg/kg,在20~500μg/kg范围内时,线性关系良好.以2 mg/kg的剂量肌肉注射2.5%头孢喹肟注射液,连续用药5 d,于最后1次给药后测定不同组织中头孢喹肟的浓度.结果表明,停药后各组织中头孢喹肟浓度逐渐下降;最后一次注射后的第4 d,肺脏、脂肪＋皮肤中已经检测不到头孢喹肟;最后一次注射后的第5天,所有组织均检测不到头孢喹肟.建议休药期为3 d.

Abstract. An HPLC method was developed for the quantitative determination of cefquinome sulphate residues in swine tissues. The HPLC system consisted of C18 column （4.6 mm × 150 mm,5 μm） and the mobile phase was 3.45 g perchlorate in 1 000 mL water-phosphates 12 mL （adjust pH to3.6 lamine）. Acetonitrile （90 ：10）, and the detection wavelength was 270 nm. Three concent ration triethlevels （20,100,500 μg/kg） of cefquinome in the blank tissues were analysed,the recovery of all samples were exceed 78 %,and the average recovery rates in muscle, liver, kidneys, lung and skin＋ fat was 81.57 %, 82.42 %,81.29 %, 83. 97 %, 78. 80 % respectively, the intra-day coefficient of variance was between 1.82 % and 6.25 %,the inter-day coefficient of variance was between 1. 11% and 6.35 %. The limit of detection （LOD） of cefquinome in tissues was 20 μg/kg. The linear ranges of cefquinome sulphate was 20-500μg/kg. Cefquinome was administered intramuscularly to swines at a dosage of 2 mg/kg for five days. The concentration of medicine in all tissues was detected after the end of the treatment. The result showed that the concentration of cefquinome in lung,skin＋fat was declined lower than LOD at the 4 d,and what in others tissues was declined lower than LOD at the 5 d. A 3-day of withdrawal time was recommended.