Al Azzam Khaldun M, Saad Bahruddin, Makahleah Ahmad, Aboul-Enein Hassan Y, Elbashir Abdalla A
Universiti Sains Malaysia, Penang, Malaysia.
Biomed Chromatogr. 2010 May;24(5):535-43. doi: 10.1002/bmc.1323.
A micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of the antiviral drugs acyclovir and valacyclovir and their major impurity, guanine, was developed. The influences of several factors (surfactant and buffer concentration, pH, applied voltage, capillary temperature and injection time) were studied. Using tyramine hydrochloride as internal standard, the analytes were all separated in about 4 min. The separation was carried out in reversed polarity mode at 28 degrees C, 25 kV and using hydrodynamic injection (15 s). The separation was effected in a fused-silica capillary 100 microm x 56 cm and a background electrolyte of 20 mM citric acid-1 M Tris solution (pH 2.75), containing 125 mM sodium dodecyl sulphate and detection at 254 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 0.1-1 microg/mL (guanine) and from 0.1 to 120 microg/mL for both valacyclovir and acyclovir. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 5.0%. The proposed method was successfully applied to the determination of the analytes in tablets and creams. From the previous study it is concluded that the stability-indicating method developed for acyclovir and valacyclovir can be used for analysis of the drug in various stability samples.
建立了一种胶束电动色谱（MEKC）方法，用于同时测定抗病毒药物阿昔洛韦和伐昔洛韦及其主要杂质鸟嘌呤。研究了几种因素（表面活性剂和缓冲液浓度、pH值、施加电压、毛细管温度和进样时间）的影响。以盐酸酪胺为内标，在约4分钟内将分析物全部分离。分离在28℃、25 kV的反相模式下进行，采用液动进样（15 s）。分离在100μm×56 cm的熔融石英毛细管中进行，背景电解质为20 mM柠檬酸-1 M Tris溶液（pH 2.75），含有125 mM十二烷基硫酸钠，并在254 nm处检测。该方法在线性、检测限和定量限、准确度、精密度和选择性方面进行了验证。校准曲线在0.1 - 1μg/mL（鸟嘌呤）范围内呈线性，伐昔洛韦和阿昔洛韦的线性范围均为0.1至120μg/mL。日内和日间迁移时间及校正峰面积的相对标准偏差均小于5.0%。所提出的方法成功应用于片剂和乳膏剂中分析物的测定。从先前的研究得出结论，所开发的阿昔洛韦和伐昔洛韦的稳定性指示方法可用于各种稳定性样品中药物的分析。
