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目的:建立UPLC-MS/MS法同时测定人血浆中雷沙吉兰(PAI)及其代谢物1-氨基茚满(1-AI)的浓度。方法:血浆样品用乙酸乙酯萃取,离心后取上清液氮气吹干,流动相复溶后进行UPLC-MS/MS测定。色谱柱:ACQUITY UPLC BEH HIL-IC色谱柱(2.1 mm×50 mm,1.7μm);流动相:乙腈-5 mmol.L-1甲酸铵含2%甲酸(90∶10,v/v);流速:0.4 mL.min-1;柱温:35℃;进样量:5μL。电喷雾离子化(ESI),正离子模式多重反应选择离子检测(MRM),PAI及内标13C3-PAI、1-AI及相应内标13C3-1-AI的检测离子对分别为m/z 172.0!117.0和175.0!120.0、m/z 134.0!117.0和137.0!120.0。结果:血浆中PAI和1-AI线性范围分别为0.02～10 ng.mL-1(r=0.9983)和0.1～50 ng.mL-1(r=0.9993)。日内、日间精密度(RSD)均小于15%,准确度(RE)均小于±15%,血浆基质对PAI和1-AI测定无干扰。结论:本研究建立的同时定量测定人血浆中PAI及1-AI的UPLC-MS/MS方法能够快速测定血浆样品,提供准确可靠的分析结果,可用于大批临床样品的分析。
OBJECTIVE: To establish a simultaneous UPLC-MS / MS method for the simultaneous determination of rasagiline (PAI) and its metabolite 1-aminoindan (1-AI) in human plasma. Methods: The plasma samples were extracted with ethyl acetate. After centrifugation, the supernatant was dried under nitrogen and the mobile phase was reconstituted for UPLC-MS / MS. Column: ACQUITY UPLC BEH HIL-IC column (2.1 mm × 50 mm, 1.7 μm); mobile phase: acetonitrile -5 mmol·L -1 ammonium formate containing 2% formic acid (90:10, v / v) : 0.4 mL.min-1; column temperature: 35 ℃; injection volume: 5μL. Electrospray ionization (ESI), positive ion mode multiple reaction selective ion detection (MRM), PAI and internal standard 13C3-PAI, 1-AI and corresponding internal standard 13C3-1-AI detection ion pairs were m / z 172.0 ! 117.0 and 175.0! 120.0, m / z 134.0! 117.0 and 137.0! 120.0. Results: The linear ranges of plasma PAI and 1-AI were 0.02-10 ng.mL-1 (r = 0.9983) and 0.1-50 ng.mL-1 (r = 0.9993), respectively. Intra-day and inter-day precision (RSD) were less than 15%, accuracy (RE) were less than ± 15%, plasma matrix on PAI and 1-AI determination without interference. Conclusion: The UPLC-MS / MS method for the simultaneous quantitative determination of PAI and 1-AI in human plasma, established in this study, can rapidly determine plasma samples and provide accurate and reliable analytical results for a large number of clinical samples.