Hussein Samiha Abd El-Rahman, El-Wadood Hanaa Mohamed Abd, Abdallah Mohamed Abou-El Wafa, Khorshed A Abd El-Hamid
Assiut University, Faculty of Pharmacy, Department of Pharmaceutical Analytical Chemistry, 71526 Assiut, Egypt.
J AOAC Int. 2015 Mar-Apr;98(2):354-60. doi: 10.5740/jaoacint.14-179.
A selective, accurate, precise, and highly sensitive HPTLC assay with reflectance/fluorescence densitometry was developed to separate and quantify some angiotensin II receptor blockers (ARBs), namely, losartan potassium, irbesartan, valsartan, and olmesartan medoxomil, in tablets and plasma. Separation of the target ARBs was performed on precoated silica gel HPTLC plates developed using chloroform-glacial acetic acid (7.5 + 2.5, v/v) mobile phase. The drugs were adequately resolved. After the exposure of the chromatograms to concentrated hydrochloric acid vapor for 10 min, the scanner was set in the reflectance/fluorescence mode with 255 nm excitation wavelength and >400 nm emission filter. The linear regression analysis data for the calibration curves of all studied drugs produced a good linear relationship with correlation coefficients ranging from 0.9991 to 0.9999 over the concentration range of 2-20 ng/band. LOD and LOQ values of all studied drugs ranged from 0.6 to 0.8 and from 1.7 to 2.4 ng/band, respectively. The developed method was successfully applied for analysis of the target ARBs in tablets and spiked human plasma samples with good precision and accuracy.
建立了一种采用反射率/荧光密度测定法的选择性、准确、精密且高灵敏度的高效薄层色谱(HPTLC)分析方法,用于分离和定量片剂及血浆中的一些血管紧张素II受体拮抗剂(ARB),即氯沙坦钾、厄贝沙坦、缬沙坦和奥美沙坦酯。在使用氯仿 - 冰醋酸(7.5 + 2.5,v/v)流动相展开的预涂硅胶HPTLC板上进行目标ARB的分离。药物得到了充分分离。将色谱图暴露于浓盐酸蒸汽中10分钟后,将扫描仪设置为反射率/荧光模式,激发波长为255 nm,发射滤光片大于400 nm。所有研究药物校准曲线的线性回归分析数据在2 - 20 ng/条带的浓度范围内呈现良好的线性关系,相关系数范围为0.9991至0.9999。所有研究药物的检测限(LOD)和定量限(LOQ)值分别为0.6至0.8 ng/条带和1.7至2.4 ng/条带。所建立的方法成功应用于片剂和加标人血浆样品中目标ARB的分析,具有良好的精密度和准确度。