用于在 HPLC-DAD 分析前从人尿中选择性分离七种磺胺类药物的Μ磁集成织物相吸附萃取(MI-FPSE)

IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Microchemical Journal Pub Date : 2024-09-01 DOI:10.1016/j.microc.2024.111552
Glykeria N. Tsompanopoulou, Abuzar Kabir, Kenneth G. Furton, Natasa P. Kalogiouri, Victoria F. Samanidou
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引用次数: 0

摘要

本研究采用磁性集成织物相吸附萃取法(MI-FPSE)从人体尿液中选择性地萃取了七种磺胺类药物(即磺胺甲基嘧啶、磺胺甲噁嗪、磺胺甲氧哒嗪、磺胺甲噁嗪、磺胺异噁唑和磺胺二甲氧嗪),然后采用高压液相色谱-二极管阵列检测法(HPLC-DAD)进行检测。在研究了影响萃取的关键参数(即:溶胶-凝胶吸附剂的类型、萃取时间、解吸时间、搅拌速率、洗脱溶剂的类型和体积、离子强度和样品基质的 pH 值)后,采用一次一因素法对 MI-FPSE 方案进行了优化。所建立的 MI-FPSE-HPLC-DAD 方法在线性、灵敏度、选择性、准确度和精密度方面都得到了验证,结果令人满意。方法的检出限(LOD)和定量限(LOQ)分别为0.02-0.04 ng/μL和0.06-0.15 ng/μL。日内和日间测定的 RSD%值分别低于 6.7 % 和 9.4 %,显示出良好的精密度。准确度采用相对回收率进行评估,所有受检分析物的相对回收率分别为 86.3-112.9%(日内研究)和 85.5-106.9%(日间研究)。使用 ComplexGAPI 指数和蓝色适用性等级指数(BAGI)考察了拟议方法的绿色特性和实用性。
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Μagnet integrated fabric phase sorptive extraction (MI-FPSE) for the selective isolation of seven sulfonamides from human urine prior to HPLC-DAD analysis
In the present study magnet integrated fabric phase sorptive extraction (MI-FPSE) was employed for the selective extraction of seven sulfonamides (i.e., sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfamethoxazole, sulfisoxazole and sulfadimethoxine) from human urine prior to their determination by high pressure liquid chromatography – diode array detection (HPLC-DAD). The MI-FPSE protocol was optimized after studying the critical parameters that affect extraction, namely: type of sol–gel sorbent, extraction time, desorption time, stirring rate, type and volume of elution solvent, the ionic strength and the pH of the sample matrix using the one-factor-at-a-time method. The developed MI-FPSE-HPLC-DAD method was validated in terms of linearity, sensitivity, selectivity, accuracy, and precision and presented satisfactory results. The limits of detection (LODs) and quantification (LOQs) ranged between 0.02–0.04 ng/μL and 0.06–0.15 ng/μL, respectively. The RSD% values of the intra-day and inter-day assays were found lower than 6.7 % and 9.4 %, respectively, showing good precision. Accuracy was assessed using percentage of relative recovery and varied from 86.3–112.9 % (intra-day study) and 85.5–106.9 % (inter-day study) for all examined analytes. The green character and practicality of the proposed method were investigated using the ComplexGAPI index and Blue Applicability Grade Index (BAGI).
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来源期刊
Microchemical Journal
Microchemical Journal 化学-分析化学
CiteScore
8.70
自引率
8.30%
发文量
1131
审稿时长
1.9 months
期刊介绍: The Microchemical Journal is a peer reviewed journal devoted to all aspects and phases of analytical chemistry and chemical analysis. The Microchemical Journal publishes articles which are at the forefront of modern analytical chemistry and cover innovations in the techniques to the finest possible limits. This includes fundamental aspects, instrumentation, new developments, innovative and novel methods and applications including environmental and clinical field. Traditional classical analytical methods such as spectrophotometry and titrimetry as well as established instrumentation methods such as flame and graphite furnace atomic absorption spectrometry, gas chromatography, and modified glassy or carbon electrode electrochemical methods will be considered, provided they show significant improvements and novelty compared to the established methods.
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