El-Enany Nahed M, Abdelal Amina A, Belal Fathalla F, Itoh Yoshinori I, Nakamura Mitsuhiro N
Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, Egypt.
Chem Cent J. 2012 Jan 26;6(1):9. doi: 10.1186/1752-153X-6-9.
Rosiglitazone (ROZ) and glimepiride (GLM) are antidiabetic agents used in the treatment of type 2 diabetes mellitus. A survey of the literature reveals that only one spectrophotometric method has been reported for the simultaneous determination of ROS and GLM in pharmaceutical preparations. However the reported method suffers from the low sensitivity, for this reason, our target was to develop a simple sensitive HPLC method for the simultaneous determination of ROZ and GLM in their combined dosage forms and plasma.
A simple reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the simultaneous determination of Rosiglitazone (ROS) and Glimepiride (GLM) in combined dosage forms and human plasma. The separation was achieved using a 150 mm × 4.6 mm i.d., 5 μm particle size Symmetry® C18 column. Mobile phase containing a mixture of acetonitrile and 0.02 M phosphate buffer of pH 5 (60: 40, V/V) was pumped at a flow rate of 1 mL/min. UV detection was performed at 235 nm using nicardipine as an internal standard. The method was validated for accuracy, precision, specificity, linearity, and sensitivity. The developed and validated method was successfully used for quantitative analysis of Avandaryl™ tablets. The chromatographic analysis time was approximately 7 min per sample with complete resolution of ROS (tR = 3.7 min.), GLM (tR = 4.66 min.), and nicardipine (tR, 6.37 min). Validation studieswas performed according to ICH Guidelines revealed that the proposed method is specific, rapid, reliable and reproducible. The calibration plots were linear over the concentration ranges 0.10-25 μg/mL and 0.125-12.5 μg/mL with LOD of 0.04 μg/mL for both compounds and limits of quantification 0.13 and 0.11 μg/mL for ROS and GLM respectively.
The suggested method was successfully applied for the simultaneous analysis of the studied drugs in their co-formulated tablets and human plasma. The mean percentage recoveries in Avandaryl™ tablets were 100.88 ± 1.14 and 100.31 ± 1.93 for ROS and GLM respectively. Statistical comparison of the results with those of the reference method revealed good agreement and proved that there were no significant difference in the accuracy and precision between the two methods respectively. The interference likely to be introduced from some co-administered drugs such as glibenclamide, gliclazide, metformine, pioglitazone and nateglinide was investigated.
罗格列酮（ROZ）和格列美脲（GLM）是用于治疗2型糖尿病的抗糖尿病药物。文献调研显示，仅有一种分光光度法被报道用于同时测定药物制剂中的ROZ和GLM。然而，该报道方法灵敏度较低，因此，我们的目标是开发一种简单灵敏的高效液相色谱法，用于同时测定其复方制剂和血浆中的ROZ和GLM。
开发并验证了一种简单的反相高效液相色谱（RP-HPLC）法，用于同时测定复方制剂和人血浆中的罗格列酮（ROS）和格列美脲（GLM）。分离采用150 mm×4.6 mm内径、5μm粒径的Symmetry® C18色谱柱。以乙腈和pH 5的0.02 M磷酸盐缓冲液（60:40，V/V）的混合物为流动相，流速为1 mL/min。采用尼卡地平作为内标，在235 nm处进行紫外检测。该方法在准确性、精密度、特异性、线性和灵敏度方面均得到验证。所开发和验证的方法成功用于文迪雅（Avandaryl™）片的定量分析。每个样品的色谱分析时间约为7分钟，ROS（保留时间tR = 3.7分钟）；GLM（tR = 4.66分钟）和尼卡地平（tR = 6.37分钟）完全分离。根据ICH指南进行的验证研究表明，所提出的方法具有特异性、快速、可靠和可重复性。校准曲线在0.10 - 25μg/mL和0.125 - 12.5μg/mL的浓度范围内呈线性，两种化合物的检测限均为0.04μg/mL，ROS和GLM的定量限分别为0.13和0.11μg/mL。
所建议的方法成功应用于同时分析所研究药物的复方片剂和人血浆。文迪雅（Avandaryl™）片中ROS和GLM的平均回收率分别为100.88±1.14和100.31±1.93。将结果与参考方法进行统计学比较，结果显示良好的一致性，证明两种方法在准确性和精密度方面无显著差异。研究了一些同时服用的药物如格列本脲、格列齐特、二甲双胍、吡格列酮和那格列奈可能引入的干扰。
