Noguchi Shoichiro, Terada Hisaya, Tamura Yukio
Nagoya City Public Health Research Institute, Nagoya, Japan.
Shokuhin Eiseigaku Zasshi. 2008 Jun;49(3):177-88. doi: 10.3358/shokueishi.49.177.
A simultaneous determination of veterinary drugs in livestock food and seafood using liquid chromatography with tandem mass spectrometry (LC/MS/MS) was developed. Veterinary drugs were extracted with 95% acetonitrile. The solution was passed through a Florisil column, and the solvent was replaced with phosphate buffer. The extract was charged on a Sep-Pak Plus C(18) mini-column and divided into 40% methanol eluate fraction and 70% acetonitrile eluate fraction. Test solutions were analyzed by LC/MS/MS with gradient elution. By using this method, 37 kinds of veterinary drugs were obtained with over 60% recovery, and quantitation was possible in cattle muscle, egg and fish. This method was inapplicable to 28 kinds of veterinary drugs. Although quantitation was not achieved, 42 other kinds of veterinary drugs can be screened. Since the limit of quantitation for this method is less than the provisional limit in general, it is useful as a screening method in residual analysis of veterinary drugs.
建立了一种使用液相色谱-串联质谱法（LC/MS/MS）同时测定畜禽食品和海产品中兽药的方法。兽药用95%乙腈提取。溶液通过弗罗里硅土柱，并用磷酸盐缓冲液替换溶剂。提取物加载到Sep-Pak Plus C(18)微型柱上，分为40%甲醇洗脱馏分和70%乙腈洗脱馏分。测试溶液通过梯度洗脱的LC/MS/MS进行分析。使用该方法，回收率超过60%可获得37种兽药，并且可以在牛肌肉、鸡蛋和鱼类中进行定量。该方法不适用于28种兽药。虽然未实现定量，但可以筛选出其他42种兽药。由于该方法的定量限一般低于暂定限量，因此作为兽药残留分析的筛选方法很有用。
