Franco Marina, Jasionowska Renata, Salvatore Elisa
Dipartimento di Chimica, Sapienza Università, 00185 Roma, Italy.
Int J Anal Chem. 2012;2012:592650. doi: 10.1155/2012/592650. Epub 2012 Mar 22.
A competitive CZE method for quality control analysis of multivitamin preparations and veterinary products containing B-group vitamins was developed. Vitamins of interest are thiamine hydrochloride (B(1)), thiamine monophosphate chloride (B(1a)), riboflavine (B(2)), riboflavine-5'monophosphate (B(2a)), nicotinamide (B(3)), d-pantothenic acid calcium salt (B(5)), pyridoxine hydrochloride (B(6)), folic acid (B(9)), and 4-aminobenzoic acid (B(10)). These analytes were separated optimizing the experimental conditions in 20 mM tetraborate buffer pH = 9.2 as a BGE (background electrolyte), on a Beckman P/ACE System MDQ instrument, using uncoated fused silica capillary. The effective capillary length was of 49.5 cm, I.D. = 50 μm, the applied voltage 20 kV and the temperature 25°C. Detection was performed by a diode array detector at 214 nm for all vitamins except B(5) (190 nm) and B(2a) (260 nm). Separation time was about 9 min. After experimental conditions optimization, the proposed method was validated. Precision of migration time and corrected peak area, linearity range, LOD and LOQ, accuracy (recovery), robustness, and ruggedness were evaluated for each analyte demonstrating the good reliability of the method. Analyses of the pharmaceutical real samples were performed and confirmed the versatility of this method.
开发了一种用于多种维生素制剂和含B族维生素的兽药产品质量控制分析的竞争性毛细管区带电泳(CZE)方法。感兴趣的维生素有盐酸硫胺素(B₁)、氯化硫胺素单磷酸酯(B₁a)、核黄素(B₂)、核黄素-5'-单磷酸酯(B₂a)、烟酰胺(B₃)、泛酸钙盐(B₅)、盐酸吡哆醇(B₆)、叶酸(B₉)和4-氨基苯甲酸(B₁₀)。在Beckman P/ACE System MDQ仪器上,使用未涂层熔融石英毛细管,以20 mM pH = 9.2的四硼酸盐缓冲液作为背景电解质(BGE),通过优化实验条件分离这些分析物。有效毛细管长度为49.5 cm,内径 = 50 μm,施加电压20 kV,温度25°C。除B₅(190 nm)和B₂a(260 nm)外,所有维生素均在214 nm处用二极管阵列检测器进行检测。分离时间约为9分钟。在优化实验条件后,对所提出的方法进行了验证。对每种分析物评估了迁移时间和校正峰面积的精密度、线性范围、检测限和定量限、准确度(回收率)、稳健性和耐用性,证明了该方法具有良好的可靠性。对药物实际样品进行了分析,证实了该方法的通用性。