Pandya Jui J, Sanyal Mallika, Shrivastav Pranav S
Department of Chemistry, School of Sciences, Gujarat University, Ahmedabad, Gujarat, India.
Department of Chemistry, St Xavier's College, Ahmedabad, Gujarat, India.
Biomed Chromatogr. 2017 Sep;31(9). doi: 10.1002/bmc.3947. Epub 2017 Feb 27.
A new, simple, accurate and precise high-performance thin-layer chromatographic method has been developed and validated for simultaneous determination of an anthelmintic drug, albendazole, and its active metabolite albendazole, sulfoxide. Planar chromatographic separation was performed on aluminum-backed layer of silica gel 60G F using a mixture of toluene-acetonitrile-glacial acetic acid (7.0:2.9:0.1, v/v/v) as the mobile phase. For quantitation, the separated spots were scanned densitometrically at 225 nm. The retention factors (R ) obtained under the established conditions were 0.76 ± 0.01 and 0.50 ± 0.01 and the regression plots were linear (r ≥ 0.9997) in the concentration ranges 50-350 and 100-700 ng/band for albendazole and albendazole sulfoxide, respectively. The method was validated for linearity, specificity, accuracy (recovery) and precision, repeatability, stability and robustness. The limit of detection and limit of quantitation found were 9.84 and 29.81 ng/band for albendazole and 21.60 and 65.45 ng/band for albendazole sulfoxide, respectively. For plasma samples, solid-phase extraction of analytes yielded mean extraction recoveries of 87.59 and 87.13% for albendazole and albendazole sulfoxide, respectively. The method was successfully applied for the analysis of albendazole in pharmaceutical formulations with accuracy ≥99.32%.
已开发并验证了一种新的、简单、准确且精密的高效薄层色谱法,用于同时测定一种驱虫药阿苯达唑及其活性代谢物阿苯达唑亚砜。使用甲苯 - 乙腈 - 冰醋酸(7.0:2.9:0.1,v/v/v)的混合物作为流动相,在硅胶60G F铝背层上进行平面色谱分离。为了定量,在225 nm处对分离的斑点进行光密度扫描。在既定条件下获得的保留因子(Rf)分别为0.76±0.01和0.50±0.01,阿苯达唑和阿苯达唑亚砜在50 - 350和100 - 700 ng/条带的浓度范围内回归曲线呈线性(r≥0.9997)。该方法在线性、特异性、准确度(回收率)、精密度、重复性、稳定性和稳健性方面进行了验证。发现阿苯达唑的检测限和定量限分别为9.84和29.81 ng/条带,阿苯达唑亚砜的检测限和定量限分别为21.60和65.45 ng/条带。对于血浆样品,分析物的固相萃取使阿苯达唑和阿苯达唑亚砜的平均萃取回收率分别为87.59%和87.13%。该方法已成功应用于药物制剂中阿苯达唑的分析,准确度≥99.32%。