Saito Koichi, Segawa Noriko, Ito Rie
Department of Analytical Chemistry, School of Pharmacy and Pharmaceutical Sciences, Hoshi University, 2-4-41, Ebara, Shinagawa-ku, Tokyo, 142-8501, Japan.
Anal Sci. 2025 Jan;41(1):85-92. doi: 10.1007/s44211-024-00675-8. Epub 2024 Sep 27.
In this study, we investigated a solid-phase dispersive extraction (SPDE) method and solid-phase derivatization method using the same solid-phase gel to extract methamphetamine (MA) from urine samples more efficiently and perform trifluoroacetic acid (TFA) derivatization for MA analysis by gas chromatography/mass spectrometry (GC/MS). N-Methylbenzylamine (NMe-BA) was added to the urine sample as a surrogate, and MA was extracted by SPDE using Oasis HLB gel as a solid-phase agent. After drying the solid-phase gel of the SPDE, anhydrous TFA was added to the MA-absorbed HLB gel in order to derivatize MA with TFA on the solid-phase, followed by elution of the TFA derivative from this gel using ethyl acetate. As a validation of the analytical method, the limit of detection (S/N = 3) and the limit of quantification (S/N > 10) of MA were 0.002 µg/mL and 0.01 µg/mL, respectively. And the average recovery rate was 97.6-100.1%, repeatability was 5.6-10.7%, and intermediate precision was 10.1-11.4% for low (0.02 µg/mL), intermediate (0.1 µg/mL), and high (1 µg/mL) concentrations of MA added in urine. The developed pretreatment method enabled continuous extraction, cleanup, and TFA derivatization of urinary MA on the same solid-phase. Thus, urinary MA can be analyzed easily, rapidly, and with high sensitivity and accuracy.
在本研究中，我们研究了一种固相分散萃取（SPDE）方法和固相衍生化方法，该方法使用相同的固相凝胶从尿液样本中更高效地提取甲基苯丙胺（MA），并通过气相色谱/质谱联用（GC/MS）对MA进行三氟乙酸（TFA）衍生化以进行分析。将N-甲基苄胺（NMe-BA）作为替代物添加到尿液样本中，使用Oasis HLB凝胶作为固相剂通过SPDE提取MA。在干燥SPDE的固相凝胶后，将无水TFA添加到吸附有MA的HLB凝胶中，以便在固相上用TFA对MA进行衍生化，随后使用乙酸乙酯从该凝胶中洗脱TFA衍生物。作为分析方法的验证，MA的检测限（S/N = 3）和定量限（S/N > 10）分别为0.002 μg/mL和0.01 μg/mL。对于尿液中添加的低（0.02 μg/mL）、中（0.1 μg/mL）和高（1 μg/mL）浓度的MA，平均回收率为97.6 - 100.1%，重复性为5.6 - 10.7%，中间精密度为10.1 - 11.4%。所开发的预处理方法能够在同一固相上对尿液中的MA进行连续提取、净化和TFA衍生化。因此，可以轻松、快速且高灵敏度和准确地分析尿液中的MA。
