Funakoshi K, Yamashita K, Chao W, Yamaguchi M, Yashiki T
Takeda Analytical Research Laboratories, Ltd., Osaka, Japan.
J Chromatogr B Biomed Appl. 1994 Oct 3;660(1):200-4. doi: 10.1016/0378-4347(94)00273-8.
A high-performance liquid chromatographic (HPLC) method is described for the determination of busulfan in human serum using on-line derivatization and column switching. Busulfan was extracted from serum with a mixture of diethyl ether and dichloromethane. After the evaporation of the organic layer, the reconstituted residue was injected into the HPLC system and busulfan was derivatized with sodium diethyldithiocarbamate on the first short column. The back-flushed derivative was then separated on the second column. Finally, after column switching, the heart-cut fraction containing the derivative was further analysed on the third column and monitored with ultraviolet absorbance detection at 278 nm. The lower limit of quantitation in serum was 10 ng/ml.
描述了一种采用在线衍生化和柱切换的高效液相色谱（HPLC）法测定人血清中的白消安。用乙醚和二氯甲烷的混合物从血清中提取白消安。有机层蒸发后，将复溶的残渣注入HPLC系统，白消安在第一根短柱上用二乙基二硫代氨基甲酸钠进行衍生化。然后将反冲得到的衍生物在第二根柱上进行分离。最后，柱切换后，含有衍生物的中心切割馏分在第三根柱上进一步分析，并用278nm的紫外吸光度检测进行监测。血清中的定量下限为10ng/ml。
