Ragab Marwa A A, El-Kimary Eman I
Faculty of Pharmacy, Department of Pharmaceutical Analytical Chemistry, University of Alexandria, El-Messalah, Alexandria 21521, Egypt.
Faculty of Pharmacy, Department of Pharmaceutical Analytical Chemistry, University of Alexandria, El-Messalah, Alexandria 21521, Egypt.
J Chromatogr A. 2017 May 12;1497:110-117. doi: 10.1016/j.chroma.2017.03.059. Epub 2017 Mar 24.
A stereoselective high performance liquid chromatographic method with diode array detection (HPLC-DAD) was introduced for S-naproxen and esomeprazole determination in tablets. The separation was achieved on a Kromasil Cellucoat chiral column using a mobile phase consisting of hexane: isopropanol: trifluoroacetic acid (TFA) (90:9.9:0.1 v/v/v). The proposed system was found to be suitable for the enantioseparation of naproxen and omeprazole biologically active isomers. After optimization of the chromatographic conditions, resolution values of 3.84 and 2.17 could be obtained for naproxen and omeprazole isomers, respectively. The method was fully validated for the determination of S-isomers of each drug in their dosage form. Also, the enentiomeric purity was determined in commercial tablet containing S-naproxen and esomeprazole. The enantiomeric purity was calculated for each drug and the chiral impurities (R-isomers) could be determined at 1% level. The method was validated and good results with respect to linearity, precision, accuracy, selectivity and robustness were obtained. The limits of detection (LOD) and quantification (LOQ) were 2.00, 6.50 and 0.10, 0.35μgmL for S-naproxen and esomeprazole, respectively.
介绍了一种采用二极管阵列检测的立体选择性高效液相色谱法（HPLC-DAD）测定片剂中S-萘普生和埃索美拉唑的含量。在Kromasil Cellucoat手性柱上进行分离，流动相由正己烷：异丙醇：三氟乙酸（TFA）（90:9.9:0.1 v/v/v）组成。结果表明，该体系适用于萘普生和奥美拉唑生物活性异构体的对映体分离。优化色谱条件后，萘普生和奥美拉唑异构体的分离度分别为3.84和2.17。该方法已针对各药物剂型中S-异构体的测定进行了全面验证。此外，还测定了含有S-萘普生和埃索美拉唑的市售片剂中的对映体纯度。计算了每种药物的对映体纯度，手性杂质（R-异构体）的测定限为1%。该方法经过验证，在线性、精密度、准确度、选择性和稳健性方面均取得了良好结果。S-萘普生和埃索美拉唑的检测限（LOD）和定量限（LOQ）分别为2.00、6.50和0.10、0.35μg/mL。
