Humbert H, Denouel J, Keller H P
Sandoz Laboratories, Pharmaceutical Research Centre, Rueil-Malmaison, France.
J Chromatogr. 1987 Nov 27;422:205-15. doi: 10.1016/0378-4347(87)80453-x.
A highly sensitive and specific column liquid chromatographic assay with electrochemical detection was developed for hydrolysed bopindolol, an active metabolite of bopindolol (Sandonorm) in human plasma. The pre-chromatographic sample preparation involved Extrelut column clean-up followed by liquid extraction of the organic extract into dilute acetic acid. Separation was on a Nucleosil ODS 3-microns column at 40 degrees C, with a phosphate buffer-methanol mobile phase. Detection was performed at +450 mV with an ESA electrochemical detector. Mepindolol was used as internal standard and quantitation was based on peak-area ratios. Total analysis time was 14 min per sample. The recovery rate of the assay was at least 70% for both compounds. A detection limit as low as 25 pg/ml, starting with 1 ml of plasma, was achieved. The day-to-day reproducibility and accuracy, checked with quality-control samples, demonstrated the reliability of this assay used by different analysts, on different chromatographic systems and over a long period of time.
建立了一种用于检测人血浆中波吲洛尔（Sandonorm）的活性代谢物——水解波吲洛尔的高灵敏度、高特异性的柱液相色谱电化学检测法。色谱前样品制备包括用埃特拉路特柱净化，然后将有机提取物液液萃取至稀醋酸中。分离在40℃下于3微米的Nucleosil ODS柱上进行，流动相为磷酸盐缓冲液-甲醇。使用ESA电化学检测器在+450 mV下进行检测。美吲哚洛尔用作内标，定量基于峰面积比。每个样品的总分析时间为14分钟。两种化合物的测定回收率均至少为70%。以1毫升血浆开始，检测限低至25 pg/ml。通过质量控制样品检查的日常重现性和准确性表明，该方法在不同分析人员、不同色谱系统上长时间使用具有可靠性。
