Brinkman U A, Welling P L, de Vries G, Scholten A H, Frei R W
J Chromatogr. 1981 Nov 6;217:463-71. doi: 10.1016/s0021-9673(00)88098-x.
Upon irradiation with short-wavelength UV light the tranquillizer demoxepam is converted into a highly fluorescent product. This reaction serves as a sensitive and selective means of detection of low levels of demoxepam in e.g., serum after separation by means of reversed-phase high-performance liquid chromatography. The effect of mobile phase composition and time of irradiation on the intensity of the fluorescence signal has been studied. A residence time of about 2 min in the post-column photochemical reactor is optimal, band broadening being efficiently suppressed (delta t ca. 1 sec) by means of air segmentation. Linear calibration graphs are obtained over a three-orders of magnitude concentration range; the detection limit for demoxepam is about 100 pg. Further work has demonstrated that detection limits of between 40 and 100 pg can also be obtained for the photoproducts of the phenothiazines fenergan, largactil, levopromazine and nedaltran. The calibration graphs show good linearity and the analysis of spiked serum samples was successful.
在用短波长紫外光照射时,安定药去甲西泮会转化为一种高荧光产物。该反应是一种灵敏且具有选择性的检测方法,可用于在例如通过反相高效液相色谱分离后的血清中检测低水平的去甲西泮。研究了流动相组成和照射时间对荧光信号强度的影响。柱后光化学反应器中的停留时间约为2分钟是最佳的,通过空气分段可有效抑制谱带展宽(Δt约为1秒)。在三个数量级的浓度范围内可获得线性校准曲线;去甲西泮的检测限约为100皮克。进一步的研究表明,对于吩噻嗪类药物非那根、氯丙嗪、左丙嗪和奈德曲班的光产物,检测限也可达到40至100皮克。校准曲线显示出良好的线性,加标血清样品的分析取得了成功。