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

气相色谱/串联质谱（GC/MS/MS）应该是一种有效的分析方法，用于检测和鉴定高污染样品中的少量药物。在这个项目中，我们试图开发敏感和具体的方法来确定人体体液中的滥用药物。我们试图检测人体体液中的哌替啶作为模型。首先以1-苯基哌啶为内标；随后，我们发现4′-哌啶苯乙酮（4′-PAP）固相萃取纯化IS效果更好。Pethidine和IS采用BondElut C_<18>筒进行纯化。吡啶和l的加样回收率为89% ~ 109%。以（哌替啶）和m/ z204 （IS）为亲本进行质谱分析；我们扫描了m/z 174 + 202（哌替啶）和162 （IS）作为子离子。采用哌替啶峰面积与IS的比值，在1.25 ~ 40 ng/ml范围内绘制全血和尿样品的校准曲线。线性几乎很好；然而，在较高的哌替啶浓度下，峰比倾向于高于校准曲线。可能的原因是电离效率的差异，因为在阱室中可能存在一些环境差异。因此，我们得出结论，氘标记的IS对于更精确的定量是必要的。研究了麻醉镇痛药戊唑嗪的含量测定方法。

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.