Elrod L, Bauer J F, Messner S L
Analytical Research Department, Abbott Laboratories, North Chicago, Illinois 60064.
Pharm Res. 1988 Oct;5(10):664-7. doi: 10.1023/a:1015983122499.
Spectinomycin dihydrochloride is determined by liquid chromatography with electrochemical detection. The drug is chromatographed on a reverse-phase Nucleosil C18 column using an eluent containing 0.02 M sodium citrate and 0.0015 M octyl sodium sulfate (pH 6.10 with perchloric acid) and acetonitrile (100:4). Detection is performed using a coulometric detector (porous carbon working electrode) at +0.85 V. The drug and primary degradation product are detectable. Detector response is linear to at least 20 micrograms/ml, which is four times the assay level. The procedure has relative standard deviations of +/- 1.21 to +/- 2.72% for three lots of bulk drug. Sensitivity is greater than 0.1 microgram/ml of spectinomycin (5 ng on column). Repeatability at this level is +/- 4.94%.
采用液相色谱-电化学检测法测定盐酸大观霉素。该药物在反相Nucleosil C18柱上进行色谱分离，使用含有0.02M柠檬酸钠和0.0015M辛基硫酸钠（用高氯酸调至pH 6.10）以及乙腈（100:4）的洗脱液。检测使用库仑检测器（多孔碳工作电极）在+0.85V下进行。该药物及其主要降解产物均可检测到。检测器响应在至少20微克/毫升范围内呈线性，这是测定水平的四倍。该方法对三批原料药的相对标准偏差为±1.21%至±2.72%。灵敏度大于0.1微克/毫升大观霉素（柱上5纳克）。在此水平下的重复性为±4.94%。
