Dalmora Sérgio Luiz, Sangoi Maximiliano da Silva, da Silva Lucélia Magalhães, Macedo Rui Oliveira, Barth Thiago
Department of Industrial Pharmacy, Federal University of Santa Maria, Santa Maria, RS, Brazil.
J Sep Sci. 2008 Jan;31(1):169-76. doi: 10.1002/jssc.200700272.
A CZE method was developed and validated for the analysis of etoricoxib in pharmaceutical dosage forms, using prilocaine as an internal standard. The CZE method was carried out on a fused-silica capillary (50 microm id, effective length 40 cm). The BGE consisted of 25 mM tris-phosphate solution at pH 2.5. The capillary temperature was maintained at 35 degrees C, the applied voltage was 25 kV, the injection was performed using the pressure mode at 50 mbar for 5 s, with detection at 234 nm using a photodiode array detector. The method was linear in the range of 2-150 microg/mL (r(2) = 0.9999). The specificity and stability-indicating capability were proven through the degradation studies and showing also that there was no interference of the excipients of the formulation. The accuracy was 99.49% with RSD of 0.66%. The limits of quantitation and detection were 2 and 0.58 microg/mL, respectively. Moreover, method validation demonstrated acceptable results for the precision, sensitivity, and robustness. The proposed method was successfully applied for the quantitative analysis of etoricoxib pharmaceutical formulations, and the results compared to the HPLC and LC-MS/MS methods, showing nonsignificant difference (p >0.05).
开发并验证了一种毛细管区带电泳（CZE）方法，用于分析药物剂型中的依托考昔，采用丙胺卡因作为内标。CZE方法在熔融石英毛细管（内径50μm，有效长度40cm）上进行。背景电解质（BGE）由pH 2.5的25mM磷酸三钠溶液组成。毛细管温度保持在35℃，施加电压为25kV，采用压力模式在50mbar下进样5s，使用光电二极管阵列检测器在234nm处进行检测。该方法在2-150μg/mL范围内呈线性（r(2)=0.9999）。通过降解研究证明了该方法的特异性和稳定性指示能力，并且还表明制剂辅料无干扰。准确度为99.49%，相对标准偏差（RSD）为0.66%。定量限和检测限分别为2和0.58μg/mL。此外，方法验证表明该方法在精密度、灵敏度和稳健性方面取得了可接受的结果。所提出的方法成功应用于依托考昔药物制剂的定量分析，结果与高效液相色谱（HPLC）和液相色谱-串联质谱（LC-MS/MS）方法相比，差异无统计学意义（p>0.05）。
