Kentzer E J, Cottingham L S, Smallidge R L
Purdue University, Department of Biochemistry, West Lafayette, IN 47907.
J Assoc Off Anal Chem. 1988 Mar-Apr;71(2):251-5.
Amprolium is extracted with methanol-water (2 + 1) containing 5mM dioctylsulfosuccinate (DOSS) and 10mM CaCl2. The analyte is separated from coextracted materials by isocratic ion-pair reverse-phase liquid chromatography, following removal of late-eluting materials on an acid alumina cleanup column, and is detected at 270 nm. The mobile phase contains 4mM DOSS with 0.3% diethylamine and 1% acetic acid in 40% acetonitrile. Linearity is satisfactory over the range of 2.5-50 micrograms/mL. Mean recovery, as determined by standard addition to commercial samples, is 100.1%. Accuracy was further tested in studies comparing the LC method to the official AOAC colorimetric method, using commercial samples, and was found to be satisfactory. Studies show that common poultry feed additives, grass meals, and some pelletization aids do not interfere with the analysis; however, when bentonite is present, recovery is decreased. The precision of the method, measured over several experiments on commercial samples, is satisfactory as indicated by coefficients of variation ranging from less than 1 to 4.5. A ruggedness test resulted in an overall CV of 3.2%, indicating the probable success of the method in a collaborative study.
用含有5mM二辛基磺基琥珀酸酯（DOSS）和10mM氯化钙的甲醇 - 水（2 + 1）提取氨丙啉。在酸性氧化铝净化柱上除去后期洗脱物质后，通过等度离子对反相液相色谱法将分析物与共提取物质分离，并在270nm处检测。流动相在40％乙腈中含有4mM DOSS、0.3％二乙胺和1％乙酸。在2.5 - 50微克/毫升范围内线性良好。通过向商业样品中加入标准品测定的平均回收率为100.1％。使用商业样品，通过将液相色谱法与官方AOAC比色法进行比较的研究进一步测试了准确性，结果令人满意。研究表明，常见的家禽饲料添加剂、草粉和一些制粒助剂不会干扰分析；然而，当存在膨润土时，回收率会降低。在对商业样品进行的多次实验中测量的该方法的精密度令人满意，变异系数范围为小于1至4.5。耐用性测试的总体变异系数为3.2％，表明该方法在协作研究中可能成功。
