Sensitive analysis for drugs-of-abuse in human body fluids by GC/MS/MS

气相色谱/串联质谱仪(GC/MS/MS)是检测和鉴定高污染样品中微量药物的有效分析方法。在这个项目中，我们试图开发灵敏和特定的方法来确定人体体液中的滥用药物。作为模型，我们试图在人体体液中检测到Pethidne。我们首先用1-苯基哌啶作为内标(IS)，后来发现4‘-哌啶基苯乙酮(4’-PAP)更适合固相萃取纯化IS。哌替啶和IS用BondElut C&lt；18&gt；小柱纯化。哌替啶和LS的回收率分别为89-109%。MS/MS分析以哌替啶和m/z 204(IS)为补充，子离子为m/z 174+202(哌替啶)和162(IS)。对于添加的全血和尿样，用度冷丁与IS的峰面积之比，在1.25~40 ng/ml的范围内绘制了校正曲线。线性关系良好；但在较高浓度的度冷丁中，峰高的比例往往高于标准曲线。可能的原因是电离效率的不同，因为在囚室中可能存在一些环境差异。因此，我们得出的结论是，为了更准确地定量，应该有必要使用氚标记的IS。我们正在努力建立一种麻醉性镇痛剂五唑西林的检测方法。

Gas chromatography / tandem mass spectrometry (GC/MS/MS) should be a useful analytical method for detecting and identifying small amounts of drugs in highly contaminated samples. In this project, we have tried to develop sensitive and specific methods for determining drugs-of-abuse in human body fluids. We tried to detect pethidne in human body fluids, as a model. We first used 1-phenylpiperidine as internal standard (IS) ; later, we found 4'-piperidinoacetophenone (4'-PAP) was better for purifying IS by solid-phase extraction. Pethidine and IS were purified using BondElut C_<18> cartridges. The recoveries were 89 - 109 % for pethidine and lS. As parentions, (pethidine) and m/z 204 (IS) were used for the MS/MS analysis; we scanned m/z 174 + 202 (pethidine) and 162 (IS) as daughter ions. For spiked whole blood and urine samples, calibration curves were drawn in the range of 1.25 - 40 ng/ml pethidine, using the ratio of peak areas of pethidine to IS. The linearity was almost good; in higher pethidine concentrations, however, the peak ratios tend to be above the calibration curve. The possible cause would be due to the differences of ionization efficiency, because some environmental difference may have existed in the trap chamber. Thus we have concluded that deuterium-labeled IS should be necessary for more precise quantitation. We are trying to develop the determination methods for pentazocine, a narcotic analgesics.