Demirkaya-Miloglu Fatma, Kadioglu Yucel, Senol Onur
Department of Analytical Chemistry, Faculty of Pharmacy, Ataturk University, 25240, Erzurum, Turkey.
Iran J Pharm Res. 2014 Spring;13(2):353-64.
was performed in both direct analysis of MSB and analysis of MN by converting MSB to MN with sodium carbonate. GC-FID method was carried out on the HP-5 capillary column GC-FID and HPLC-DAD methods were developed for determination of menadione (MN) and menadione sodium bisulphite (MSB). By means of each method, quantitative analysis of MSB in commercial pharmaceutical using nitrogen gas. HPLC-DAD method was achieved on the reversed phase C8 column by using a mobile phase consisting methanol and water. The calibration curves of GC-FID and HPLC-DAD for both analytes were linear in the same concentration range (0.5-20 μg/mL). Both methods were validated in terms of precision, accuracy, recovery and limits of detection (LOD) and quantitation (LOQ). Although LOD values of HPLC-DAD method (0.010 μg/mL for MN and 0.005 μg/mL for MSB) is lower than obtained values with GC-FID method (0.04 μg/mL for MN and 0.06 μg/mL for MSB), both methods gave similar and favorable results in terms of precision and accuracy. The Student's t-test was applied to investigate the significant of the different between the results of MSB determination with direct analysis of MSB and analysis of MN by converting MSB to MN by means of GC-FID and HPLC-DAD method in dosage form.
对亚硫酸氢钠甲萘醌（MSB）进行直接分析以及通过用碳酸钠将MSB转化为甲萘醌（MN）来分析MN。在HP-5毛细管柱上进行气相色谱-火焰离子化检测（GC-FID）方法，并且开发了高效液相色谱-二极管阵列检测（HPLC-DAD）方法用于测定甲萘醌（MN）和亚硫酸氢钠甲萘醌（MSB）。通过每种方法，使用氮气对市售药品中的MSB进行定量分析。HPLC-DAD方法是在反相C8柱上通过使用由甲醇和水组成的流动相来实现的。两种分析物的GC-FID和HPLC-DAD校准曲线在相同浓度范围（0.5 - 20μg/mL）内呈线性。两种方法在精密度、准确度、回收率以及检测限（LOD）和定量限（LOQ）方面都进行了验证。尽管HPLC-DAD方法的LOD值（MN为0.010μg/mL，MSB为0.005μg/mL）低于GC-FID方法获得的值（MN为0.04μg/mL，MSB为0.06μg/mL），但两种方法在精密度和准确度方面都给出了相似且良好的结果。应用学生t检验来研究在剂型中通过MSB直接分析和通过GC-FID以及HPLC-DAD方法将MSB转化为MN来分析MN的结果之间差异的显著性。
