Sunaric Slavica, Petkovic Milica, Denic Marko, Mitic Snezana, Pavlovic Aleksandra
University of Nis, Faculty of Medicine, Department of Chemistry, Bulevar dr Zorana Djindjica 81,18000 Nis, Serbia.
Acta Pol Pharm. 2013 May-Jun;70(3):403-11.
Solid-phase extraction method followed by direct UV spectrophotometry at 264 nm was developed and applied for the selective ibuprofen determination in two-component formulation of ibuprofen and pseudoephedrine-HCl, combined powder which contains ibuprofen in the form of salt with L-arginine and 10% ibuprofen cream. Procedures for ibuprofen determination in complex pharmaceutical preparations by direct UV spectrophotometry lack selectivity because of interferences of other active substances and fat components. A limited number of spectrophotometric methods applicable to these samples are based on derivative (first and second-order) UV spectroscopy. Common HPLC procedures are more selective but more expensive and for creams also require some type of extraction because the large amount of oily excipients would clog up the column. The proposed solid-phase extraction method proved to be suitable for analysis of ibuprofen in combined tablets, powders and creams by direct UV spectrophotometry. Also the method provides an effective clean-up of the cream and allows ibuprofen determination by HPLC analysis. For the extraction three different commercial sorbents were tested: anion exchange Oasis MAX, hydrophilic-lipophilic balanced Oasis HLB and reverse-phase Chromabond C18ec. The optimization of the SPE method was first done on standard ibuprofen solutions and then the suitability of the method was checked on solutions of commercial pharmaceutical samples. The method yields good results for all three types of commercial preparations on the anion-exchange Oasis MAX cartridges, with recoveries of 90-100.2%. The interferences in UV analysis were not registered and good precision (RSD < 6%) was obtained. The present method has been verified as accurate as the reference HPLC with the great advantage of less expensive instrumentation. For this reason, the method would be suitable for a routine and rapid drug quality control.
开发了一种固相萃取方法，随后在264nm处进行直接紫外分光光度法，用于测定布洛芬与盐酸伪麻黄碱的两组分制剂、含L-精氨酸盐形式布洛芬的复方粉末以及10%布洛芬乳膏中的布洛芬。由于其他活性物质和脂肪成分的干扰，采用直接紫外分光光度法测定复方药物制剂中布洛芬的方法缺乏选择性。适用于这些样品的分光光度法数量有限，基于导数（一阶和二阶）紫外光谱。常见的高效液相色谱法选择性更强，但成本更高，对于乳膏还需要某种类型的萃取，因为大量油性赋形剂会堵塞色谱柱。所提出的固相萃取方法被证明适用于通过直接紫外分光光度法分析复方片剂、粉末和乳膏中的布洛芬。该方法还能有效净化乳膏，并可通过高效液相色谱分析测定布洛芬。为了萃取，测试了三种不同的市售吸附剂：阴离子交换Oasis MAX、亲水亲油平衡的Oasis HLB和反相Chromabond C18ec。首先在标准布洛芬溶液上对固相萃取方法进行优化，然后在市售药物样品溶液上检查该方法的适用性。该方法在阴离子交换Oasis MAX柱上对所有三种类型的市售制剂都能产生良好的结果，回收率为90 - 100.2%。未发现紫外分析中的干扰，精密度良好（相对标准偏差<6%）。本方法已被验证与参考高效液相色谱法一样准确，且具有仪器成本较低的巨大优势。因此，该方法适用于常规和快速的药物质量控制。
