Solangi Amber R, Bhanger Muhammad I, Memon Saima Q, Khuhawar Muhammad Y, Mallah Arfana
University of Sindh, National Center of Excellence in Analytical Chemistry, Jamshoro, Pakistan.
J AOAC Int. 2009 Sep-Oct;92(5):1382-9.
A simple, sensitive, and novel method has been developed and validated for the separation and simultaneous quantitation of seven structurally different drugs-pipemidic acid and ofloxacin quinolone antibiotics, pseudoephedrine decongestant, piroxicam anti-inflammatory, thiamin, pyridoxine, and cobalamin-in a mixture by capillary zone electrophoresis. Factors affecting the separation were pH, concentration of buffer, and applied voltage. Separation was carried out in < 9 min with a 50 mM sodium tetraborate buffer, pH 10, and an applied voltage of 30 kV in an uncoated silica capillary tube. The carrier electrolyte gave baseline separation with good resolution, reproducibility, and accuracy. Calibration plots were linear over at least three orders of magnitude of analyte concentrations, and the lower LODs were within the range of 1-5 microg/mL. Detection was performed by UV absorbance at 230 nm. The method was validated for the analysis of drugs in pharmaceutical preparations and in urine samples with RSD of 0.5-2.4% and recovery of > 99%.
已开发并验证了一种简单、灵敏且新颖的方法,用于通过毛细管区带电泳分离并同时定量混合物中的七种结构不同的药物——吡哌酸和氧氟沙星喹诺酮类抗生素、伪麻黄碱减充血剂、吡罗昔康抗炎药、硫胺素、吡哆醇和钴胺素。影响分离的因素有pH值、缓冲液浓度和施加电压。在未涂层的石英毛细管中,使用pH值为10的50 mM四硼酸钠缓冲液和30 kV的施加电压,在不到9分钟内完成分离。载流电解质实现了基线分离,具有良好的分辨率、重现性和准确性。校准曲线在至少三个数量级的分析物浓度范围内呈线性,最低检测限在1 - 5 μg/mL范围内。通过在230 nm处的紫外吸光度进行检测。该方法经过验证,可用于分析药物制剂和尿液样本中的药物,相对标准偏差为0.5 - 2.4%,回收率大于99%。