Belal Fathalla, Omar Mahmoud A, Derayea Sayed, Hammad Mohamed A, Zayed Sahar, Saleh Safaa F
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
Department of Analytical Chemistry, Faculty of Pharmacy, Minia University, Minia, Egypt.
J Chromatogr Sci. 2018 Mar 1;56(3):233-241. doi: 10.1093/chromsci/bmx105.
A simple, sensitive and rapid micellar liquid chromatographic method was developed and validated for simultaneous determination of four drugs, namely, paracetamol (PAR), tizanidine (TZD), aceclofenac (ACF) and nimesulide (NMD). Good chromatographic separation was achieved using Cyano column and micellar mobile phase consisting of 120 mM sodium dodecyl sulfate, 25 mM phosphate buffer and 10% (V/V) butanol. The pH was adjusted to three using phosphoric acid. The total retention time was below 10 min. The analysis was performed at a flow rate of 1 mL/min and a column temperature of 40°C with direct UV detection at 230 nm. Diclofenac sodium was used as the internal standard. The proposed method was validated according to the ICH guidelines and was successfully applied to the analysis of these drugs in their tablet dosage forms with high accuracy. Limits of detection were found to be 0.03, 0.07, 0.033 and 0.11 μg/mL for PAR, ACF, TZD and NMD, respectively. The high sensitivity of developed method permitted its application to the in-vitro determination of the cited drugs in spiked human plasma and urine samples, and the obtained results were satisfactory. However, PAR could not be determined in spiked human urine because its peak overlapped with that of the urine peak.
建立并验证了一种简单、灵敏且快速的胶束液相色谱法，用于同时测定四种药物，即对乙酰氨基酚（PAR）、替扎尼定（TZD）、醋氯芬酸（ACF）和尼美舒利（NMD）。使用氰基柱和由120 mM十二烷基硫酸钠、25 mM磷酸盐缓冲液和10%（V/V）丁醇组成的胶束流动相实现了良好的色谱分离。用磷酸将pH值调至3。总保留时间在10分钟以下。分析在流速为1 mL/min、柱温为40°C的条件下进行，采用230 nm的直接紫外检测。双氯芬酸钠用作内标。所提出的方法根据国际协调会议（ICH）指南进行了验证，并成功应用于这些药物片剂剂型的分析，具有很高的准确性。PAR、ACF、TZD和NMD的检测限分别为0.03、0.07、0.033和0.11 μg/mL。所开发方法的高灵敏度使其能够应用于加标人血浆和尿液样本中上述药物的体外测定，获得的结果令人满意。然而，PAR无法在加标人尿液中测定，因为其峰与尿液峰重叠。
