Rahimi Marzieh, Bahar Soleiman, Amininasab S Mojtaba
Department of Chemistry, Faculty of Science, University of Kurdistan, P.O. Box 416, Sanandaj, Iran.
J Anal Methods Chem. 2022 Jul 13;2022:9027920. doi: 10.1155/2022/9027920. eCollection 2022.
This study reports the construction of a novel SPME fiber based on chitosan and glutaraldehyde as coating material composites combined with high-performance liquid chromatography with an ultraviolet detector (HPLC-UV) for extraction and detection of phenobarbital. In this technique, the chitosan biopolymer, as a new coating of SPME fiber, was produced on the stainless-steel wire, using glutaraldehyde and phenobarbital as cross-linker and template, respectively. For comparison, a nonimprinted polymer was created using the same procedure to evaluate fiber selectivity (but without the addition of phenobarbital). The SPME-MIP fiber coating was characterized by field emission scanning electron microscopy, Fourier-transform infrared spectroscopy, and thermal gravimetric analysis. The efficiency of fiber was then improved by adjusting the impact of numerous factors such as pH, extraction time, desorption time, desorption solvent, and stirring rate. The results showed that the proposed fiber has a linear range of 0.01-4 g·mL, and detection limit of 7.5 ng·mL. The average recoveries in the four concentration levels for the spiked river and well water samples were 95.7 and 95.3%, with relative standard deviations of 3.8 and 5.9% for single fiber and between fibers, respectively.
本研究报道了一种新型固相微萃取(SPME)纤维的构建,该纤维以壳聚糖和戊二醛为涂层材料复合材料,结合配备紫外检测器的高效液相色谱法(HPLC-UV)用于苯巴比妥的萃取和检测。在该技术中,壳聚糖生物聚合物作为SPME纤维的新涂层,分别以戊二醛和苯巴比妥为交联剂和模板,在不锈钢丝上制备而成。为作比较,采用相同程序制备了一种非印迹聚合物以评估纤维的选择性(但不添加苯巴比妥)。通过场发射扫描电子显微镜、傅里叶变换红外光谱和热重分析对SPME-分子印迹聚合物(MIP)纤维涂层进行了表征。然后通过调整pH、萃取时间、解吸时间、解吸溶剂和搅拌速率等多种因素的影响来提高纤维的效率。结果表明,所提出的纤维线性范围为0.01 - 4 g·mL,检测限为7.5 ng·mL。加标河水和井水样品在四个浓度水平下的平均回收率分别为95.7%和95.3%,单根纤维和不同纤维之间的相对标准偏差分别为3.8%和5.9%。