Şule Temiz, Songül Ulusoy, Halil İbrahim Ulusoy, Esra Durgun, Ümmügülsüm Polat, Gökhan Sarp
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引用次数: 0
Abstract
A new sample preparation and determination method, including HPLC-DAD analysis after Magnetic Solid Phase Extraction (MSPE), was developed to monitor the trace amounts of two types of nonsteroidal anti-inflammatory drugs (NSAIDs), Ibuprofen (IBP) and Ketoprofen (KP). In the proposed method, IBP and KP analytes were extracted from newly synthesized magnetic-based sorbent in a pH 4.0 buffer medium and enriched by desorbing again with ethanol to a smaller volume before chromatographic determinations. The samples were filtered and transferred to HPLC vials before analysis. The experimental variables were optimized step by step such as adsorption time, desorption solvent, pH, etc. After preconcentration of IBP and KP molecules by MSPE, determination of target molecules was carried out by isocratic elution of 30 % Methyl alcohol, 40 % Trifluoro Acetic Acid (TFA) (0.1 %, v:v), 30 % Acetonitrile. By using optimized conditions, the detection limits of target molecules were calculated as 3.43 ng mL-1 and 3.48 ng mL-1 for IBP and KP, respectively. The triplicate measurements made with model solutions containing 100 ng mL-1 of target molecules, RSD %values were found below 3.50 %. The developed method was successfully applied to synthetic urine and pooling urine samples. Finally, the practicality and suitability for green analytical chemistry of the proposed method was evaluated by using Blue Applicability Grade Index (BAGI) and Green Analytical Procedure Index (GAPI).
采用磁固相萃取(MSPE)后HPLC-DAD分析方法,建立了布洛芬(IBP)和酮洛芬(KP)两种非甾体类抗炎药(NSAIDs)的检测方法。在该方法中,IBP和KP分析物在pH 4.0的缓冲介质中从新合成的磁基吸附剂中提取,并在色谱测定前再次用乙醇解吸到更小的体积。样品经过过滤后转移到HPLC瓶中进行分析。对吸附时间、解吸溶剂、pH等实验参数进行了逐步优化。用MSPE预富集IBP和KP分子后,用30%甲醇、40%三氟乙酸(0.1%,v:v)、30%乙腈等密度洗脱法测定目标分子。通过优化条件,计算出IBP和KP的检出限分别为3.43 ng mL-1和3.48 ng mL-1。用含100 ng mL-1目标分子的模型溶液进行三次测量,RSD %值均低于3.50%。该方法已成功地应用于合成尿液和尿液样本池。最后,采用蓝色适用性等级指数(BAGI)和绿色分析程序指数(GAPI)对所提方法的实用性和绿色分析化学适用性进行了评价。
期刊介绍:
The Journal of Chromatography B publishes papers on developments in separation science relevant to biology and biomedical research including both fundamental advances and applications. Analytical techniques which may be considered include the various facets of chromatography, electrophoresis and related methods, affinity and immunoaffinity-based methodologies, hyphenated and other multi-dimensional techniques, and microanalytical approaches. The journal also considers articles reporting developments in sample preparation, detection techniques including mass spectrometry, and data handling and analysis.
Developments related to preparative separations for the isolation and purification of components of biological systems may be published, including chromatographic and electrophoretic methods, affinity separations, field flow fractionation and other preparative approaches.
Applications to the analysis of biological systems and samples will be considered when the analytical science contains a significant element of novelty, e.g. a new approach to the separation of a compound, novel combination of analytical techniques, or significantly improved analytical performance.