Determination of Residual Isometamidium in Cattle Tissues and Milk by HPLC
Determination of Residual Isometamidium in Cattle Tissues and Milk by HPLC
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DOI：
10.3358/shokueishi.40.3_211
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发表时间：
1999-06
期刊：
影响因子：
--
通讯作者：
K. Kondo;M. Horie;M. Murayama;Takashi Suzuki;M. Toyoda
中科院分区：
文献类型：
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作者：
K. Kondo;M. Horie;M. Murayama;Takashi Suzuki;M. Toyoda
建立了牛肌肉、肝脏、脂肪和牛奶中抗三体药物异美他定（IMD）的高效液相色谱测定方法。样品经乙腈-0.25mol/L甲酸铵甲醇溶液提取，乙酸乙酯-水液液分配，再用乙腈在氯化钠存在下萃取水层。蒸发乙腈后，将残留物溶于1 mL 0.25 mol/L甲酸铵甲醇溶液中。采用高效液相色谱法，在380 nm处检测，使用辛基柱（TSK-GEL Octyl-80 Ts，4.6mm i.流动相为乙腈-0.03mol/L柠檬酸（含0.005mol/L庚烷磺酸钠）（3：7）。当添加0.1μg/g IMD时，牛肌肉、肝脏、脂肪和牛奶中药物的回收率分别为76.0%、75.3%、88.0%和89.0%。检出限为0.01μg/g。还研究了通过LC/MS分析IMD。
A determination method for the antitripanosomal agent, isometamidium (IMD) in cattle muscle, liver, fat and milk has been developed by using HPLC. The drug was extracted from a sample with acetonitrile-0.25mol/L ammonium formate methanol solution, and purified by liquid-liquid partition with ethyl acetate and water, followed by extraction of the water layer in the presence of NaCl with acetonitrile. After evaporation of acetonitrile, the residue was taken up in 1mL of 0.25mol/L ammonium formate methanol solution. The drug was determined by HPLC with detection at 380nm using an octyl column (TSK-GEL Octyl-80Ts, 4.6mm i. d.×150mm), and acetonitrile-0.03mol/L citric acid containing 0.005mol/L sodium 1-heptanesulfonate (3:7) as an eluent. Recoveries of the drug from cattle muscle, liver, fat and milk were 76.0, 75.3, 88.0 and 89.0%, respectively, when 0.1μg/g of IMD was spiked. The detection limit was 0.01μg/g. The analysis of IMD by LC/MS was also investigated.