Robertson D L, Butterfield A G, Kolasinski H, Lovering E G, Matsui F F
J Pharm Sci. 1979 May;68(5):577-80. doi: 10.1002/jps.2600680516.
A quantitative high-performance liquid chromatographic method for the determination of chlorpropamide, tolbutamide, and their respective hydrolysis products, p-chlorobenzenesulfonamide and p-toluenesulfonamide, in solid dosage forms was developed. The method is stability indicating and can be used to determine the sulfonamide hydrolysis product and the intact drug in the presence of minor degradates. Method reproducibility, demonstrated by repeated injections of a calibration standard, was 1.21%. The lower limit of quantitation of the hydrolysis products, p-chlorobenzenesulfonamide and p-toluenesulfonamide, was 0.2 microgram/5-microliter injection. The accuracy of the method for intact drugs was determined by comparison of the HPLC results to those obtained by the appropriate USP or BP assays. The mean of the results obtained by the two methods differed by 0.7% for chlorpropamide and 0.3% for tolbutamide. Pure drug samples were spiked with amounts of the hydrolysis products ranging from 20 to 120% of the intact content. The mean percent recovery for p-chlorobenzenesulfonamide was 98.6%; for p-toluenesulfonamide, it was 100.6%. A qualitative TLC procedure for the detection of chlorpropamide, p-chlorobenzenesulfonamide, dipropylurea, propylurea, n-propylamine, tolbutamide, p-toluenesulfonamide, dibutylurea, butylurea, and n-butylamine is also described.
建立了一种用于测定固体剂型中氯磺丙脲、甲苯磺丁脲及其各自水解产物对氯苯磺酰胺和对甲苯磺酰胺的定量高效液相色谱法。该方法具有稳定性指示作用，可用于在存在少量降解产物的情况下测定磺酰胺水解产物和完整药物。通过重复进样校准标准品证明的方法重现性为1.21%。水解产物对氯苯磺酰胺和对甲苯磺酰胺的定量下限为0.2微克/5微升进样量。通过将高效液相色谱结果与通过适当的美国药典或英国药典分析获得的结果进行比较，确定了该方法对完整药物的准确性。两种方法获得的结果平均值，氯磺丙脲相差0.7%，甲苯磺丁脲相差0.3%。向纯药物样品中加入含量范围为完整含量20%至120%的水解产物。对氯苯磺酰胺的平均回收率为98.6%；对甲苯磺酰胺的平均回收率为100.6%。还描述了一种用于检测氯磺丙脲、对氯苯磺酰胺、二丙基脲、丙基脲、正丙胺、甲苯磺丁脲、对甲苯磺酰胺、二丁基脲、丁基脲和正丁胺的定性薄层色谱法。
