Adams A K, Essien H, Binder S R
Clinical HPLC Group, Bio-Rad Laboratories, Hercules, CA 94547.
Ann Biol Clin (Paris). 1991;49(5):291-7.
This paper describes the application of an automated algorithm for drug identification following the liquid chromatographic on-line separation and purification of drugs in physiological fluids. Two hundred fifty-seven (257) drugs and 45 drug metabolites were assembled for testing. Two internal standards were used which monitored different columns in the multi-step analytical separation. Retention reproducibility over a nine month period was 4 p. cent or less for most drugs. The algorithm for matching unknown peaks against the stored library utilized relative retention, lambda maxima, normalized spectral overlays, wavelength ratios and zero-intercepts from the second derivative in a combined forward-reverse search. Most of the drugs which could not be unambiguously identified were sedatives which eluted in the first minutes of the chromatogram. Diasteromers were partially resolved. Repetitive analysis of 200-400 micrograms/l of amphetamine, diphenhydramine, imipramine and morphine were evaluated to establish an absorption cutoff of 12 mAbs, above which at least 95% of peaks were correctly identified. This corresponded to a signal-to-noise ratio of 12 for the scanning UV detector which was evaluated.
本文描述了一种自动算法在生理体液中药物液相色谱在线分离与纯化后进行药物鉴定的应用。收集了257种药物和45种药物代谢物用于测试。使用了两种内标物，它们在多步分析分离中监测不同的色谱柱。在九个月的时间里，大多数药物的保留重现性为4%或更低。将未知峰与存储库进行匹配的算法在正向-反向联合搜索中利用了相对保留时间、最大吸收波长、归一化光谱叠加、波长比和二阶导数的零截距。大多数无法明确鉴定的药物是在色谱图开始几分钟内洗脱的镇静剂。非对映异构体得到了部分分离。对200 - 400微克/升的苯丙胺、苯海拉明、丙咪嗪和吗啡进行了重复分析，以确定12 mAbs的吸收截止值，高于该值时至少95%的峰能被正确鉴定。这对应于所评估的扫描紫外检测器的信噪比为12。
