Kizu R, Hayakawa K, Miyazaki M
Faculty of Pharmaceutical Sciences, Kanazawa University, Japan.
Biomed Chromatogr. 1989 Jan;3(1):14-9. doi: 10.1002/bmc.1130030105.
A method for determining cis-diamminedichloroplatinum(II) (CDDP), an anticancer drug, in plasma and urine by HPLC with UV detection and column-switching has been developed. Typical conditions were as follows. An apparatus was composed of two columns, two pumps, a UV detector, a sample injector with a 100 microL loop, a switching valve, a column oven and a recorder. A Rheodyne model 7125 sample injector was used as the switching valve. A precolumn (4.6 mm ID x 25 cm) was packed with MCI GEL CK10S (a strong cation exchanger), and an analytical column (4.6 mm ID x 5 cm) was packed with MCI GEL CDR10 (a strong anion exchanger). Both columns were connected in series via the switching valve. The CDDP-containing fraction of the effluent from the precolumn was loaded to the analytical column by column-switching and the effluent from the analytical column was monitored at 210 nm. An eluent of 0.3 M sodium dihydrogen phosphate was pumped at a flow rate of 1 mL/min and the columns were maintained at 40 degrees C. CDDP was eluted at about 11 min and the identity of the peak of CDDP on the chromatogram was confirmed by its 3-dimensional chromatogram and analysis of platinum in the column effluent. Under the conditions described above, a linear relationship was obtained between peak height and concentration of CDDP up to 100 microM. Correlation efficients were 0.998 for plasma and 0.999 for urine. The detection limit was 0.1 microM for CDDP in both plasma and urine (S/N = 3,0.005 AUFS). The reproducibility was within 3% for 10 determinations.(ABSTRACT TRUNCATED AT 250 WORDS)
已开发出一种通过带紫外检测和柱切换的高效液相色谱法测定血浆和尿液中抗癌药物顺二氨二氯铂(II)(CDDP)的方法。典型条件如下。仪器由两根色谱柱、两个泵、一个紫外检测器、一个带有100微升定量环的进样器、一个切换阀、一个柱温箱和一个记录仪组成。使用Rheodyne 7125型进样器作为切换阀。预柱(内径4.6毫米×25厘米)填充有MCI GEL CK10S(强阳离子交换剂),分析柱(内径4.6毫米×5厘米)填充有MCI GEL CDR10(强阴离子交换剂)。两根色谱柱通过切换阀串联连接。通过柱切换将预柱流出物中含CDDP的部分加载到分析柱上,并在210纳米处监测分析柱的流出物。以0.3 M磷酸二氢钠为洗脱液,流速为1毫升/分钟,色谱柱保持在40℃。CDDP在约11分钟时洗脱,通过其三维色谱图和柱流出物中铂的分析确认色谱图上CDDP峰的一致性。在上述条件下,CDDP峰高与浓度在高达100微摩尔范围内呈线性关系。血浆的相关系数为0.998,尿液的相关系数为0.999。血浆和尿液中CDDP的检测限均为0.1微摩尔(信噪比=3,0.005 AUFS)。10次测定的重现性在3%以内。(摘要截短为250字)