Park Jin-Hee, Park Yoo-Sin, Rhim Si-Youn, Kim Hyun-Jin, Jhee Ok-Hwa, Lee Yun-Sik, Lee Min-Ho, Shaw Leslie M, Kang Ju-Seop
Department of Pharmacology and Institute of Biomedical Sciences, College of Medicine, Hanyang University, Seoul, South Korea.
Biomed Chromatogr. 2009 Dec;23(12):1350-6. doi: 10.1002/bmc.1260.
A rapid and validated method for analysis of levosulpiride in human plasma using liquid chromatography coupled to tandem mass spectrometry was developed. Levosulpiride and tiapride (IS, internal standard) were extracted from alkalized plasma samples with ethylacetate and separation by RP-HPLC. Detection was performed by positive ion electrospray ionization in multiple-reaction monitoring mode, monitoring the transitions m/z 342.1 --> m/z 112.2 and m/z 329.1 --> m/z 213.2, for quantification of levosulpiride and IS, respectively. The standard calibration curves showed good linearity within the range of 2-200 ng/mL (r(2) > or = 0.9990). The lower limit of quantitation was 2 ng/mL. The retention times of levosulpiride (0.63 min) and IS (0.66 min) presented a significant time saving benefit of the proposed method. No significant metabolic compounds were found to interfere with the analysis. This method offered good precision and accuracy and was successfully applied for the pharmacokinetic and bioequivalence study of a 25 mg of levosulpiride tablet in 24 healthy Korean volunteers.
建立了一种快速且经过验证的使用液相色谱-串联质谱法分析人血浆中左舒必利的方法。左舒必利和硫必利（内标，IS）从碱化的血浆样品中用乙酸乙酯萃取，并通过反相高效液相色谱法分离。采用正离子电喷雾电离在多反应监测模式下进行检测，分别监测m/z 342.1→m/z 112.2和m/z 329.1→m/z 213.2的跃迁，以定量左舒必利和内标。标准校准曲线在2 - 200 ng/mL范围内显示出良好的线性（r(2)≥0.9990）。定量下限为2 ng/mL。左舒必利（0.63分钟）和内标的保留时间（0.66分钟）表明该方法具有显著的省时优势。未发现明显的代谢化合物干扰分析。该方法具有良好的精密度和准确性，并成功应用于24名健康韩国志愿者中25 mg左舒必利片的药代动力学和生物等效性研究。
