Skinner M, Kanfer I
School of Pharmaceutical Sciences, Rhodes University, Grahamstown, South Africa.
J Chromatogr. 1988 Dec 28;459:261-7. doi: 10.1016/s0021-9673(01)82035-5.
A high-performance liquid chromatographic assay for the analysis of josamycin in human serum and urine is presented. The assay involves a simple solid-phase extraction procedure coupled with a phase separation step, separation on a reversed-phase C18 column with UV detection by a multi-wavelength programmable detector. The mobile phase was acetonitrile-0.015 M phosphate buffer, pH 6.0 (5:2) at a flow-rate of 1.2 ml/min. The column temperature was maintained at 35 degrees C. Linear calibration curves over the concentration ranges 0.1-2.0 mg/l (serum) and 0.5-5 mg/l (urine) were obtained with correlation coefficients of 0.9983 and 1.0000, respectively. The relative standard deviations of five replicate samples at the upper and lower limits of each calibration curve were below 7%. The recoveries at the upper and lower ends of the calibration range for serum were 77% and 70%, respectively, and those for urine were 76% and 80%, respectively.
本文介绍了一种用于分析人血清和尿液中交沙霉素的高效液相色谱法。该方法包括一个简单的固相萃取程序以及一个相分离步骤，在反相C18柱上进行分离，通过多波长可编程检测器进行紫外检测。流动相为乙腈-0.015M磷酸盐缓冲液（pH 6.0，5:2），流速为1.2 ml/min。柱温保持在35℃。在0.1 - 2.0 mg/l（血清）和0.5 - 5 mg/l（尿液）的浓度范围内获得了线性校准曲线，相关系数分别为0.9983和1.0000。每个校准曲线上下限处五个重复样品的相对标准偏差均低于7%。血清校准范围上下端的回收率分别为77%和70%，尿液的回收率分别为76%和80%。
