Ramisetti Nageswara Rao, Bompelli Sravan
Analytical Chemistry Division, Discovery Laboratory, Indian Institute of Chemical Technology, Tarnaka, Hyderabad, 500 607, India.
Biomed Chromatogr. 2014 Dec;28(12):1846-53. doi: 10.1002/bmc.3229. Epub 2014 May 10.
A simple and selective polar ionic liquid chromatography-tandem mass spectrometric method for separation and determination of cinacalcet enantiomers in rat plasma was developed and validated. The chromatographic separation was accomplished on a Chirobiotic V column packed with vancomycin as a chiral stationary phase using 2.5 mm ammonium formate in 100% methanol as a mobile phase in an isocratic mode of elution at a flow rate of 1.0 mL/min. The analytes were extracted from rat plasma by precipitating the proteins with acetonitrile. The developed method exhibited a linear dynamic range over 0.5-500 ng/mL in rat plasma for both enantiomers. The method was successfully applied to study the pharmacokinetics after a single dose by oral administration of 10 mg/kg of cinacalcet enantiomers to healthy male Wistar rats.
建立并验证了一种简单且具有选择性的极性离子液体色谱-串联质谱法,用于分离和测定大鼠血浆中的西那卡塞对映体。色谱分离在填充有万古霉素作为手性固定相的Chirobiotic V柱上进行,以100%甲醇中2.5 mM甲酸铵为流动相,采用等度洗脱模式,流速为1.0 mL/min。通过用乙腈沉淀蛋白质从大鼠血浆中提取分析物。所建立的方法在大鼠血浆中两种对映体的线性动态范围均为0.5-500 ng/mL。该方法成功应用于对健康雄性Wistar大鼠口服10 mg/kg西那卡塞对映体单剂量后的药代动力学研究。