Iwaki K, Okumura N, Yamazaki M
School of Pharmacy, Hokuriku University, Ishikawa, Japan.
J Chromatogr. 1993 Sep 22;619(2):319-23. doi: 10.1016/0378-4347(93)80124-m.
A rapid and accurate determination of tetracycline antibiotics in human serum by reversed-phase high-performance liquid chromatography with fluorescence detection has been developed, based on protein precipitation in serum. Various reagents for precipitation were investigated, and 24% trichloroacetic acid in methanolic solution gave the maximum recovery (at least 94.3%) and interference-free chromatograms of different three tetracyclines. At a concentration of 0.5 micrograms/ml, the precision (relative standard deviation) ranged from 1.12 to 1.94%. In the range 0.04-10.0 micrograms/ml for oxytetracycline and chlorotetracycline and 0.01-10.0 micrograms/ml for tetracycline, linear responses were observed. The detection limits of this method were 10-35 ng/ml for all three antibiotics. The proposed method was applied to the determination of serum concentrations in subjects receiving tetracycline antibiotics.
基于血清中的蛋白质沉淀，开发了一种采用反相高效液相色谱荧光检测法快速准确测定人血清中四环素类抗生素的方法。研究了各种沉淀试剂，甲醇溶液中24%的三氯乙酸给出了最大回收率（至少94.3%），且不同的三种四环素均得到无干扰的色谱图。浓度为0.5微克/毫升时，精密度（相对标准偏差）范围为1.12%至1.94%。土霉素和金霉素在0.04 - 10.0微克/毫升范围内，四环素在0.01 - 10.0微克/毫升范围内，观察到线性响应。该方法对所有三种抗生素的检测限为10 - 35纳克/毫升。所提出的方法应用于接受四环素类抗生素治疗的受试者血清浓度的测定。
