猪组织中硫酸头孢喹肟含量测定和肌注给药残留研究

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.

Detemination cefquinome sulphate in swine tissues and residues after intramuscular injection

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 with triethlamine):Acetonitrile(90∶10),and the detection wavelength was 270 nm.Three concentration levels(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 20～500 μg/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.