Dewani A P, Tripathi A S, Shelke P G, Bakal R L, Mohale D S, Chandewar A V
Department of Quality Assurance, Pataldhamal Wadhwani College of Pharmacy, Yavatmal, India.
Department of Pharmacology, Pataldhamal Wadhwani College of Pharmacy, Yavatmal, India.
J Chromatogr Sci. 2017 Mar 1;55(3):327-333. doi: 10.1093/chromsci/bmw189.
A novel, simple and mass spectrometry (MS) compatible high-performance liquid chromatography (HPLC) method is reported for the simultaneous estimation of ilaprazole (ILA) and glimepiride (GLM) in rat plasma. The bio-analytical procedure involves extraction of ILA, GLM and internal standard (IS) from rat plasma with a solid-phase extraction (SPE) process. The chromatographic analysis was performed on Waters-600 system using an isocratic mobile phase comprising methanol:water (80:20 % v/v) with pH of water modified to three using formic acid at a flow rate of 1.0 mL/min and Kinetex C18 column maintained at 30 ± 1°C. The signals were monitored using a PDA detector set at 225 nm. IS, ILA and GLM eluted at 2.04, 4.7 and 7.4 min, respectively, and the total run time was 10 min. Method validation was performed as per US Food and Drug Administration guidelines and the results met the acceptance criteria. The calibration curve was linear over a concentration range of 10-600 ng/mL (r2 = 0.999). The intra- and inter-day precisions for ILA and GLM were (%RSD values) in the range of 1.52-9.74 and 1.52-11.76%, respectively, in rat plasma. The method was successfully applied in pharmacokinetic studies followed by oral administration of GLM and ILA in rats.
报道了一种新颖、简单且与质谱（MS）兼容的高效液相色谱（HPLC）方法，用于同时测定大鼠血浆中的伊拉普唑（ILA）和格列美脲（GLM）。生物分析程序包括通过固相萃取（SPE）过程从大鼠血浆中提取ILA、GLM和内标（IS）。色谱分析在Waters - 600系统上进行，使用等度流动相，该流动相由甲醇：水（80:20 % v/v）组成，用甲酸将水的pH调节至3，流速为1.0 mL/min，Kinetex C18柱保持在30 ± 1°C。使用设置在225 nm的PDA检测器监测信号。IS、ILA和GLM分别在2.04、4.7和7.4分钟洗脱，总运行时间为10分钟。按照美国食品药品监督管理局的指南进行方法验证，结果符合验收标准。校准曲线在10 - 600 ng/mL的浓度范围内呈线性（r2 = 0.999）。大鼠血浆中ILA和GLM的日内和日间精密度（%RSD值）分别在1.52 - 9.74%和1.52 - 11.76%范围内。该方法成功应用于大鼠口服GLM和ILA后的药代动力学研究。
