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目的:建立测定兔血浆和组织中辣椒碱(capsaicin,CAP)和二氢辣椒碱(dihydrocapsaicin,DHC)浓度的LC-MS/MS法。方法:100μL血浆或组织样品经液-液萃取后,以乙腈-0.1%甲酸(70∶30)为流动相,经Agilent Extend C18柱(150 mm×2.1 mm,5μm)分离,采用电喷雾电离源,以多反应监测(MRM)方式进行正离子检测。用于定量分析的离子分别为m/z 306.4→m/z 137.3(CAP),m/z 308.2→m/z 137.3(DHC)和m/z 494.0→m/z 369.1(内标格列本脲)。结果:测定血浆和组织中CAP和DHC的线性范围均为0.125~50 ng·m L-1,最低定量限(LLOQ)均为0.125 ng·m L-1。日内、日间精密度(RSD)均±15.0%,准确度(RE)均在±11.5%以内。结论:该方法专属性强、灵敏度高、快速,可同时测定兔血浆和组织中CAP和DHC的浓度,适用于CAP和DHC的药动学研究。
OBJECTIVE: To establish a LC-MS / MS method for the determination of capsaicin (CAP) and dihydrocapsaicin (DHC) concentrations in rabbit plasma and tissues. METHODS: 100 μL plasma or tissue samples were separated by liquid-liquid extraction using acetonitrile-0.1% formic acid (70:30) as mobile phase on an Agilent Extend C18 column (150 mm × 2.1 mm, 5 μm) , With multiple reaction monitoring (MRM) for positive ion detection. The ions used for the quantitative analysis were m / z 306.4 → m / z 137.3 (CAP), m / z 308.2 → m / z 137.3 (DHC) and m / z 494.0 → m / z 369.1 ). RESULTS: The linear range of determination of CAP and DHC in plasma and tissue was 0.125 ~ 50 ng · m L-1, and the lowest limit of quantitation (LLOQ) was 0.125 ng · m L-1. The intraday and interday precision (RSD) were ± 15.0% and the accuracy (RE) was within ± 11.5%. Conclusion: This method is specific, sensitive and rapid. It can measure the concentration of CAP and DHC in plasma and tissue of rabbits at the same time. It is suitable for pharmacokinetic study of CAP and DHC.