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磷酸替米考星在猪组织中的残留消除研究
刘彩1, 沈向荣1, 杨迪1, 张晓辉1, 宗昕如1, 王文超2, 鲍恩东1
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(1.南京农业大学动物医学院, 南京 210095;2.宁夏泰瑞制药股份有限公司, 银川 750001)
摘要:
为了解磷酸替米考星在猪肌肉、肝脏、肾脏、皮肤和脂肪等组织中的残留消除规律,制订安全合理的药物休药期,利用高效液相色谱法(HPLC)在280 nm处检测10%磷酸替米考星可溶性粉的代谢物替米考星在猪组织中的残留情况,对HPLC检测方法进行改良,确定流动相体积比为乙腈:四氢呋喃:二丁胺磷酸盐缓冲液:水=10:5:5:80。测得猪肝、肾中替米考星的检测限为0.025 μg/g,定量限为0.05 μg/g,肌肉、脂肪和皮肤中替米考星的检测限为0.01 μg/g,定量限为0.02 μg/g;平均加标回收率为77.56%~97.82%,变异系数为0.78%~10.5%。以80 mg/L临床推荐剂量进行饮水给药,连续7 d,在肝、肾组织中药物残留量较高,在肌肉、皮肤和脂肪中残留量较低。使用休药期WT1.4软件计算,替米考星在肝脏的休药期为5.73 d,在肾脏的休药期为3.75 d,在肌肉的休药期为11.57 d,在皮肤和脂肪的休药期为10.91 d,按双单侧95%置信区间计算替米考星在猪的休药期为12 d。
关键词:    磷酸替米考星  HPLC  残留
DOI:10.11841/j.issn.1007-4333.2013.04.21
投稿时间:2012-11-30
基金项目:江苏高校优势学科建设工程资助项目(PAPD)
Study on residue depletion of tilmicosin phosphate in swine tissues
LIU Cai1, SHEN Xiang-rong1, YANG Di1, ZHANG Xiao-hui1, ZONG Xin-ru1, WANG Wen-chao2, BAO En-dong1
(1.Nanjing Agricultural University, College of Veterinary Medicine, Nanjing 210095, China;2.Ningxia Tairui Pharmaceutical Company Limited, Yinchuan 750001, China)
Abstract:
This purpose of this research is to study the tissue residues of the tilmicosin phosphate in swine and determine the withdrawal time.A high-performance liquid chromatography (HPLC) method with detection at 280 nm was used and validated for the determination of 10% tilmicosin phosphate soluble powder residues in pig tissues.The mobile phase was composed of acetonitrile,tetrahydrofuran,hosphate buffer and water with the volume ratio of 10:5:5:80.The limits of detection (LOD) was 0.025 μg/g,and the limits of quantitation (LOQ) was 0.05 μg/g for liver and kidney;theLODwas 0.01 μg/g and the LOQ was 0.02 μg/g for muscle,fat and skin.Average recoveries ranged from 77.56% to 97.82%,coefficient of variance ranged from 0.78% to 10.5%.Administrated over 7-day by 80 mg/L of Tilmicosin Phosphate in drinking water,the residue levels were higher in liver and kidney,and lower in muscle,fat and skin.According to the calculation by software WT1.4,the withdrawal period of tilmicosin residues is 5.73 d in liver,3.75 d in kidney,11.57 d in muscle,10.91 d in skin and fat.It is concluded that the expected withdrawal period of tilmicosin phosphate for swine should be 12 days.
Key words:  swine  tilmicosin phosphate  HPLC  residues