Atila Alptug, Ozturk Murat, Kadioglu Yucel, Halici Zekai, Turkan Didar, Yayla Muhammed, Un Harun
Ataturk University, Department of Analytical Chemistry, Faculty of Pharmacy, Erzurum 25240, Turkey.
Turkish Public Health Association, Directorate of Erzurum, Erzurum 25100, Turkey.
J Pharm Biomed Anal. 2014 Aug;97:33-8. doi: 10.1016/j.jpba.2014.03.039. Epub 2014 Apr 4.
A rapid, simple and sensitive UFLC-MS/MS method was developed and validated for the determination of bosentan in rat plasma using etodolac as an internal standard (IS) after liquid-liquid extraction with diethyl ether-chloroform (4:1, v/v). Bosentan and IS were detected using electrospray ionization in positive ion multiple reaction monitoring mode by monitoring the transitions m/z 551.90→201.90 and 288.20→172.00, respectively. Chromatographic separation was performed on the inertsil ODS-4 column with a gradient mobile phase, which consisted of 0.1% acetic acid with 5mM ammonium acetate in water for solvent A and 5mM ammonium acetate in acetonitrile-methanol (50:50, v/v) for solvent B at a flow rate of 0.3mL/min. The method was sensitive with 0.5ng/mL as the lower limit of quantitation (LLOQ) and the standard calibration curve for bosentan was linear (r>0.997) over the studied concentration range (0.5-2000ng/mL). The proposed method was fully validated by determining specificity, linearity, LLOQ, precision and accuracy, recovery, matrix effect and stability. The validated method was successfully applied to plasma samples obtained from rats.
建立了一种快速、简单且灵敏的超高效液相色谱-串联质谱(UFLC-MS/MS)方法,以依托度酸为内标,用乙醚-氯仿(4:1,v/v)液液萃取后,用于测定大鼠血浆中的波生坦。采用电喷雾电离,在正离子多反应监测模式下分别监测m/z 551.90→201.90和288.20→172.00的跃迁,对波生坦和内标进行检测。在Inertsil ODS-4柱上进行色谱分离,流动相为梯度洗脱,其中A相为含0.1%乙酸和5mM乙酸铵的水溶液,B相为含5mM乙酸铵的乙腈-甲醇(50:50,v/v)混合溶液,流速为0.3mL/min。该方法灵敏度高,定量下限(LLOQ)为0.5ng/mL,在所研究的浓度范围(0.5 - 2000ng/mL)内,波生坦的标准校准曲线呈线性(r>0.997)。通过测定特异性、线性、LLOQ、精密度、准确度、回收率、基质效应和稳定性,对所提出的方法进行了全面验证。该验证方法成功应用于从大鼠获得的血浆样本。