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Electrochemically deposition of ionic liquid modified graphene oxide for circulated headspace in-tube solid phase microextraction of naphthalene from honey samples followed by on-line liquid chromatography analysis.
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2020-08-13 , DOI: 10.1016/j.chroma.2020.461486
Shahram Seidi 1 , Hadis Abolhasani 1 , Yasaman Razeghi 1 , Maryam Shanehsaz 2 , Mahshid Manouchehri 1
Affiliation  

In this work, an inexpensive, fast, and selective ionic liquid modified graphene oxide (GO-IL) was synthesized and electrochemically deposited on the inner surface of a stainless-steel tube. Then, it was applied for circulated headspace in-tube solid-phase microextraction (CHS-IT-SPME) of naphthalene from honey samples. Next, the coated tube was replaced with the sample loop of a six-port injection valve for on-line desorption and further HPLC-UV analysis of naphthalene. The sorbent was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FT-IR), and energy-dispersive X-ray spectroscopy (EDX). Different parameters affecting the procedure efficiency, including extraction temperature, extraction time, salt concentration, and sample volume were optimized by central composite design and response surface methodology. Under the optimum conditions, the calibration curve was linear within the range of 0.3-200 ng mL-1, with a regression coefficient of 0.9972. The limits of detection (LOD) and quantification (LOQ) were found to be 0.1 ng mL-1 and 0.3 ng mL-1, respectively. Intra-day and inter-day RSDs% for three replicate measurements of naphthalene at the concentration of 10 ng mL-1 were obtained 3.9% and 5.0%, respectively. Also, good tube-to-tube reproducibility of 5.3% was achieved. Finally, the method was successfully applied for measuring trace amounts of naphthalene in honey samples. Relative recoveries were calculated within the range of 90.0-106.5%, indicating excellent efficiency of the proposed method.



中文翻译:

电化学沉积离子液体修饰的氧化石墨烯,用于从蜂蜜样品中循环顶空管内固相微萃取萘,然后进行在线液相色谱分析。

在这项工作中,廉价,快速,选择性离子液体改性氧化石墨烯(GO-IL)合成并电化学沉积在不锈钢管的内表面。然后,将其应用于蜂蜜样品中萘的循环顶空管内固相微萃取(CHS-IT-SPME)。接下来,将涂覆的试管替换为六端口进样阀的样品定量环,以进行在线脱附并进一步进行萘的HPLC-UV分析。通过扫描电子显微镜(SEM),透射电子显微镜(TEM),傅立叶变换红外光谱(FT-IR)和能量色散X射线光谱(EDX)对吸附剂进行表征。影响程序效率的不同参数,包括提取温度,提取时间,盐浓度,通过中央复合设计和响应面方法优化了样本量。在最佳条件下,校准曲线在0.3-200 ng mL范围内呈线性-1,回归系数为0.9972。检出限(LOD)和定量限(LOQ)分别为0.1 ng mL -1和0.3 ng mL -1。在浓度为10 ng mL -1的情况下,对萘进行三份重复测量的日内和日间RSDs%分别为3.9%和5.0%。同样,获得了良好的5.3%的管到管重现性。最终,该方法成功应用于蜂蜜样品中痕量萘的测定。计算的相对回收率在90.0-106.5%的范围内,表明该方法的效率极高。

更新日期:2020-08-15
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