Wang Ying, Zhao Guan-An, Li Xia, Zhang En, Tan Wei, Chen Jia-Qi
Department of Pharmacy, The Affiliated Lihuili Hospital, Ningbo University, Ningbo, Zhejiang, China.
Urinary Surgery, The People's Hospital of Lishui, Lishui, Zhejiang, China.
Front Pharmacol. 2023 Aug 28;14:1211383. doi: 10.3389/fphar.2023.1211383. eCollection 2023.
A fast, simple, and sensitive ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established for the quantification of safinamide in rat plasma. Plasma samples were treated with acetonitrile for protein precipitation, and diazepam was used as an internal standard (IS). The analytes were separated on an Acquity UPLC C18 (2.1 mm × 50 mm, 1.7 μm) chromatographic column with gradient elution using a mobile phase (0.1% formic acid-acetonitrile). Then, the eluates were detected by electrospray ionization (ESI) in positive ion mode. The analytes were quantified by multiple reaction monitoring (MRM) using the transition m/z 303.3→215.0 of safinamide and m/z 285.0→154.0 of IS. Safinamide had good linearity in the concentration range of 1.0-2000 ng/mL, and the lower limit of quantitation (LLOQ) was 1.0 ng/mL. The intra- and inter-day precision and accuracy of safinamide were less than 7.63%, while the average recovery rate was 92.98%-100.29%. The method was validated to be stable and had low noise, short chromatographic run time, wide linear range, small sample volumes, low sample injection volumes, and high sensitivity. Therefore, it can be used in pharmacokinetics and preclinical and clinical studies.
建立了一种快速、简便、灵敏的超高效液相色谱串联质谱法（UPLC-MS/MS）用于定量大鼠血浆中的沙芬酰胺。血浆样品用乙腈进行蛋白沉淀处理，地西泮用作内标（IS）。分析物在Acquity UPLC C18（2.1 mm×50 mm，1.7μm）色谱柱上分离，采用流动相（0.1%甲酸-乙腈）进行梯度洗脱。然后，洗脱液在正离子模式下通过电喷雾电离（ESI）进行检测。分析物通过多反应监测（MRM）进行定量，采用沙芬酰胺的m/z 303.3→215.0和内标的m/z 285.0→154.0的跃迁。沙芬酰胺在1.0 - 2000 ng/mL浓度范围内具有良好的线性，定量下限（LLOQ）为1.0 ng/mL。沙芬酰胺的日内和日间精密度及准确度均小于7.63%，平均回收率为92.98% - 100.29%。该方法经验证具有稳定性，噪声低，色谱运行时间短，线性范围宽，样品体积小，进样量低，灵敏度高。因此，可用于药代动力学以及临床前和临床研究。
