Sangoi Maximiliano da Silva, Wrasse Micheli, D'Avila Felipe Bianchini, Bernardi Raquel Martini, de Oliveira Paulo Renato, Dalmora Sérgio Luiz, Bueno Rolim Clarice Madalena
Faculty of Pharmacy, Federal University of Rio Grande do Sul, 90610-000 Porto Alegre-RS, Brazil.
Eur J Mass Spectrom (Chichester). 2009;15(6):723-30. doi: 10.1255/ejms.1044.
A simple, specific, rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of fluticasone propionate (FP) in pharmaceutical formulations was developed and validated using deflazacort as internal standard (IS). The LC-MS/MS method was carried out on a C8 column (50 mm) with a mobile phase consisted of methanol : water (95 : 5, v/v) 100 mM formic acid-50 mM ammonium acetate (90 : 5 : 5, v/v/v). The mass spectrometry method was performed employing positive atmospheric pressure chemical ionization technique, operating in multiple reaction monitoring mode. The chromatographic separation was obtained within 1.5 min and it was linear in the concentration range of 10-1000 ng mL(-1). Moreover, method validation demonstrates acceptable results for the specificity, accuracy, precision and robustness. The proposed method was successfully applied for the quantitative analysis of FP nasal sprays and the results were compared to validated liquid chromatography and capillary electrophoresis methods with photodiode array detectors showing non-significant difference (P > 0.05).
建立了一种简单、特异、快速且灵敏的液相色谱-串联质谱(LC-MS/MS)法,以地夫可特为内标(IS),用于分析药物制剂中的丙酸氟替卡松(FP),并进行了方法验证。该LC-MS/MS法在一根50 mm的C8柱上进行,流动相由甲醇:水(95:5,v/v)、100 mM甲酸-50 mM乙酸铵(90:5:5,v/v/v)组成。质谱法采用正大气压化学电离技术,在多反应监测模式下运行。1.5分钟内实现了色谱分离,在10 - 1000 ng mL(-1)浓度范围内呈线性。此外,方法验证表明该方法在特异性、准确性、精密度和稳健性方面均获得了可接受的结果。所提出的方法成功应用于FP鼻喷雾剂的定量分析,并将结果与经验证的配备光电二极管阵列检测器的液相色谱法和毛细管电泳法进行比较,结果显示无显著差异(P > 0.05)。