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

通过 GC/MS/MS 对人体体液中的滥用药物进行灵敏分析

• 批准号: 12670391
• 负责人: ISHII Akira
• 金额: $ 2.05万
• 依托单位: NAGOYA UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 2000
• 资助国家: 日本
• 起止时间: 2000 至 2001
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-12670391/
• 关键词: Gas chromatography; Tandem mass spectrometry; Pethidine; Solid-phase extraction; Codeine; Pentazocine

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.

气相色谱/串联质谱法（GC/MS/MS）应该是一种有用的分析方法，用于检测和鉴定高度污染样品中的少量药物。在这个项目中，我们试图开发灵敏和特异的方法来确定人体体液中的滥用药物。我们尝试在人体体液中检测哌替啶，作为一个模型。我们先用1-苯基哌啶作内标物，后来发现用4 ′-哌啶基苯乙酮（4 ′-PAP）作内标物，用固相萃取法提纯内标物效果较好。使用BondElut C_柱纯化哌替啶和IS<18>。哌替啶和1 S的回收率为89 - 109%。作为括号，（哌替啶）和m/z 204（IS）用于MS/MS分析;我们扫描了m/z 174 + 202（哌替啶）和162（IS）作为子离子。对于加标全血和尿液样本，使用哌替啶与IS的峰面积比，在1.25 - 40 ng/ml哌替啶范围内绘制校准曲线。线性几乎良好;然而，在较高的哌替啶浓度下，峰比往往高于校准曲线。可能的原因是由于电离效率的差异，因为可能存在一些环境差异的陷阱室。因此，我们得出结论，氘标记的IS应该是必要的更精确的定量。本文对麻醉性镇痛药喷他佐辛的含量测定方法进行了研究。

项目成果

R.Kurihara: "Simple extraction of gamma-hydroxybutylate in human whole blood by headspace soild-phase microextraction"Japanese Journal of Forensic Toxicology. 19. 38-45 (2000)

R.Kurihara：“通过顶空固相微萃取简单提取人全血中的 γ-羟基丁酯”《日本法医毒理学杂志》。

T.Yamamoto: "The application of minisatellite variant repeat mapping by PCR (MVR-PCR) in a paternity case showing false exclusion due to STR mutation"Journal of Forensic Sciences. 46. 374-378 (2001)

T.Yamamoto：“PCR (MVR-PCR) 小卫星变异重复定位在亲子鉴定案例中的应用，显示由于 STR 突变造成的错误排除”《法医科学杂志》。

Seno, H, Hattori, BL, Ishii, A., Kumazawa, T., Watanabe-Suzuki, K, Suzuki, O.: "Analyses of butyrophenones and their analogues in whole blood by high-performance liquid chromatographyelectrospray tandem mass spectrometry"J. Chromatogr. B. 746. 3-9 (2000)

Seno, H, Hattori, BL, Ishii, A., Kumazawa, T., Watanabe-Suzuki, K, Suzuki, O.：“通过高效液相色谱电喷雾串联质谱法分析全血中的丁酰苯及其类似物”J

Ishii, A., Kurihara, R., Watanabe-Suzuki, K, Kumazawa, T., Seno, H., Matsushima H, Suziki O, Katsumata Y.: "Sensitive determination of pethidine in body fluids by surface ionization organic mass spectrometry"J. Cromatogr. B. 758. 117-121 (2001)

Ishii, A., Kurihara, R., Watanabe-Suzuki, K, Kumazawa, T., Seno, H., Matsushima H, Suziki O, Katsumata Y.：“通过表面电离有机质谱法灵敏测定体液中哌替啶

M. Mizutani: "Analysis of 168 short tandem repeat loci in the Japanese population, using a screening set for human genetic mapping"Journal of Human Genetics. 46. 448-455 (2001)

M. Mizutani：“使用人类遗传图谱筛选集分析日本人群中的 168 个短串联重复基因座”《人类遗传学杂志》。