Graham R E, Kenner C T, Biehl E R
J Pharm Sci. 1975 Jun;64(6):1013-7. doi: 10.1002/jps.2600640628.
Iodochlorhydroxyquin was separated from various corticosteroids using an acetonitrile-diatomaceous earth column. Iodochlorhydroxyquin was eluted with cyclohexane, and the corticosteroid was eluted with chloroform. Iodochlorhydroxyquin was determined by both a UV absorbance method and a new compleximetric method using the nickel chelate of iodochlorhydroxyquin. The corticosteroid was determined by the blue tetrazolium and isoniazid procedures. The average percent recovery for these four methods was 100.8, 99.4,100.7, and 99.9, respectively, for 10 known mixtures. The standard deviation for the absorbance for 10 determinations of the nickel complex was 0.002 absorbance unit (0.31%). Various characteristics of the nickel and other complexes were evaluated, including the sensitivity, solubility, and wavelength of maximum absorbance in 14 different solvents. The analyses of 23 typical products are reported, for which the standard deviation, expressed as a percentage of the amount declared, was 1.31% for the UV, 1.34% for the compleximetric, 1.49% for the blue tetrazolium, and 1.22% for the isoniazid procedures. Methods of determination in the presence of interferences are discussed.
采用乙腈 - 硅藻土柱从多种皮质类固醇中分离出氯碘羟喹。氯碘羟喹用环己烷洗脱，皮质类固醇用氯仿洗脱。氯碘羟喹通过紫外吸光法和使用氯碘羟喹镍螯合物的新络合滴定法测定。皮质类固醇通过蓝四氮唑法和异烟肼法测定。对于10种已知混合物，这四种方法的平均回收率分别为100.8%、99.4%、100.7%和99.9%。镍络合物10次测定吸光度的标准偏差为0.002吸光度单位（0.31%）。评估了镍络合物和其他络合物的各种特性，包括在14种不同溶剂中的灵敏度、溶解度和最大吸收波长。报告了对23种典型产品的分析结果，其中以申报量的百分比表示的标准偏差，紫外法为1.31%，络合滴定法为1.34%，蓝四氮唑法为1.49%，异烟肼法为1.22%。讨论了在有干扰情况下的测定方法。
