Hanna G M, Lau-Cam C A
U.S. Food and Drug Administration, New York Regional Laboratory, Brooklyn 11232.
J AOAC Int. 1993 May-Jun;76(3):526-30.
A simple, specific, and accurate proton nuclear magnetic resonance (1H-NMR) spectroscopic method has been developed for the identification and assay of furosemide and its degradation product, 4-chloro-5-sulfamoylanthranilic acid (CSA), in tablets and injections. Dissolution of the sample in D2O-NaOD resulted in a solution yielding the required separation among the resonance signals of furosemide, CSA, and tert-butyl alcohol, the internal standard. The mean +/- SD recovery values of furosemide and CSA from 10 synthetic formulations were 99.6 +/- 0.8 and 98.9 +/- 1.7%, respectively. Commercial tablets (6 lots) and injections (5 lots) of furosemide were assayed by the proposed method and found to contain 53.1-99.8% furosemide and 0.3-45.2% CSA.
已开发出一种简单、特异且准确的质子核磁共振（1H-NMR）光谱法，用于片剂和注射剂中呋塞米及其降解产物4-氯-5-氨磺酰基邻氨基苯甲酸（CSA）的鉴别和含量测定。将样品溶解于D2O-NaOD中，得到的溶液能使呋塞米、CSA和内标叔丁醇的共振信号实现所需分离。10个合成制剂中呋塞米和CSA的平均回收率（均值±标准差）分别为99.6±0.8%和98.9±1.7%。采用所提出的方法对呋塞米的6批市售片剂和5批注射剂进行了含量测定，结果发现其中呋塞米含量为53.1-99.8%，CSA含量为0.3-45.2%。
