Rashid Ahmad Junaid, Bashir Sajid, Bukhari Nadeem Irfan, Abbas Nasir, Raza Atif, Munir Ans, Ijaz Qazi Aamir, Akbar Shehla, Arshad Numera, Ishtiaq Saiqa
Faculty of Pharmacy, Department of Pharmaceutics, University of Sargodha, Sargodha, Pakistan.
University College of Pharmacy, University of the Punjab, Lahore, Pakistan.
Pak J Pharm Sci. 2021 Jul;34(4(Supplementary)):1629-1637.
A simple, sensitive and precise high performance liquid chromatographic (HPLC) method was developed and validated for determination of flavoxate HCI in raw material, tablets and biological fluids. The method followed by using the Zorbax XDB-C18 column containing Di-isobutyl n-octadeceylsilane (4.6mm×150mm, 5μm). The mobile phase consisted of acetonitrile: methanol: 0.15M sodium perchlorate (17:35:48 v/v) having pH 3. UV detection was carried out at 229nm at 40°C. Results indicated that the method has successfully established and validated in accordance with ICH guidelines acceptance criteria for linearity (0.03-7.5μg), accuracy (101.18-101.28%), robustness of column age and column lot (peak area %CV<0.04, purity %CV< 0.006) and robustness of HPLC condition (%CV<0.02), precision (intra and inter day precision assay, %CV values for peak area and percent purity of flavoxate HCl<2%) and system suitability parameters. The average noise, theoretical LOD and LOQ were found to be 0.01 mAU, 0.03 mAU and 0.6ng, respectively. The Coefficient of determination (r2) ranging from 0.03μg to 7.5μg, 0.99 which was within acceptable criteria of r & gt 0.99. The spiked recoveries of samples were 101.28, 101.18 and 101.18% respectively. All data revealed that this method can be used for in-vitro & in-vivo determination of flavoxate HCI in various pharmaceutical preparations.
建立了一种简单、灵敏、准确的高效液相色谱（HPLC）法，用于测定原料药、片剂和生物样品中的盐酸黄酮哌酯，并进行了方法验证。该方法采用含二异丁基正十八烷基硅烷的Zorbax XDB-C18柱（4.6mm×150mm，5μm）。流动相由乙腈：甲醇：0.15M高氯酸钠（17:35:48 v/v）组成，pH值为3。在40℃下于229nm处进行紫外检测。结果表明，该方法已成功建立并按照国际人用药品注册技术协调会（ICH）指南的接受标准进行了验证，包括线性（0.03 - 7.5μg）、准确度（101.18 - 101.28%）、柱龄和柱批次的稳健性（峰面积%CV<0.04，纯度%CV<0.006）以及HPLC条件的稳健性（%CV<0.02）、精密度（日内和日间精密度测定，盐酸黄酮哌酯峰面积和纯度百分比的%CV值<2%）和系统适用性参数。平均噪声、理论检测限和定量限分别为0.01 mAU、0.03 mAU和0.6ng。在0.03μg至7.5μg范围内的决定系数（r2）为0.99，在r>0.99的可接受标准范围内。样品的加标回收率分别为101.28%、101.18%和101.18%。所有数据表明，该方法可用于各种药物制剂中盐酸黄酮哌酯的体外和体内测定。
