Fink D W, Martin R P, Pivnichny J V, Shim J S
J Assoc Off Anal Chem. 1978 Sep;61(5):1078-82.
An analytical method has been developed for the determination of arprinocid (9-(2-chloro-6-fluorophenylmethyl)-9H-purin-6-amine) in feed, based upon measurement of the absorbance of the diazo chromophore formed from a product of zinc reduction of the drug in acidic solution. The analyte is extracted from the feed into chloroform in the presence of a pH 7 phosphate buffer and isolated by adsorption chromatography on alumina, followed by partitioning between hexane and 0.15M HCl. The reduction product in the aqueous phase is then treated for colorimetric measurement. This procedure has been applied to determining 0.0010--0.0080% arprinocid in feed with a precision of less than 5% relative standard deviation near the middle of this concentration range. Of 32 feed additives examined, only zoalene and sulfamethazine were serious interferences. A study and discussion of several factors, e.g., reaction time, pH, and amount of zinc metal, that affect the analytical reactions are also included.
已开发出一种用于测定饲料中阿普立西（9-(2-氯-6-氟苄基)-9H-嘌呤-6-胺）的分析方法，该方法基于对药物在酸性溶液中经锌还原产物形成的重氮发色团吸光度的测量。在pH 7的磷酸盐缓冲液存在下，将分析物从饲料中萃取到氯仿中，然后通过在氧化铝上的吸附色谱法进行分离，接着在己烷和0.15M盐酸之间进行分配。然后对水相中的还原产物进行比色测定。该方法已应用于测定饲料中0.0010--0.0080%的阿普立西，在该浓度范围中间附近，相对标准偏差小于5%。在所检测的32种饲料添加剂中，只有二氯喹啉酸和磺胺二甲嘧啶有严重干扰。文中还对影响分析反应的几个因素，如反应时间、pH值和锌金属用量等进行了研究和讨论。
