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首页> 外文期刊>Microchemical Journal: Devoted to the Application of Microtechniques in all Branches of Science >Determination of tetracycline and cefotaxime residues in honey by micro solid phase extraction based on electrospun nanofibers coupled with HPLC
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Determination of tetracycline and cefotaxime residues in honey by micro solid phase extraction based on electrospun nanofibers coupled with HPLC

机译:基于HPLC耦合的电纺纳米纤维微固相萃取测定蜂蜜四环素和头孢噻肟残留物

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In the present study, electrospun polyethylene terephthalate nanofibers doped with graphene oxide nano particles (GO-PET) was fabricated and used as an effective adsorbent in micro-solid phase extraction (mu-SPE) of tetracycline (TC) and cefotaxime (CF) from honey samples prior to HPLC. The UV-vis spectrophotometer was utilized in the optimization step. The adsorbent was fully characterized using SEM, FT-IR, BET, and BJH methods. The specific surface area and average pore size of the adsorbent were 79.5 m(2) g(-1) and 4.83 nm, respectively. The honey samples were dissolved in water (5% w/v) at 50 degrees C for 10 min, centrifuged at 4000 rpm for 15 min and finally filtered using a filter paper before performing the extraction. The important factors of the method were studied to obtain the optimal conditions. Under the optimum conditions (sample solution, 100 mL; adsorbent, 40 mg; pH 5; extraction time, 10 min; desorption solvent; MeOH, 200 mu L), the limits of detection for TC and CF were 15.3 and 3.0 mu g kg(-1). The linear dynamic range (LDR) was obtained as 10-5000 mu g kg(-1) with the determination coefficients (R-2) of 0.9939 and 0.9959, respectively. The real sample extraction recoveries were 89-94% and 95-98% for TC and CF, respectively. The intra-day and inter-day precisions were 5.6 and 4.9% (n = 3) for TC, and 3.6 and 4.5% (n = 9) for CF.
机译:在本研究中,制备掺杂有石墨烯纳米颗粒(GO-PET)的电纺聚乙烯对苯二甲酸乙二醇酯,并用作四环素(TC)和CFotaxime(CF)的微固相萃取(MU-SPE)中的有效吸附剂HPLC之前的蜂蜜样品。在优化步骤中使用UV-Vis分光光度计。使用SEM,FT-IR,BET和BJH方法完全表征吸附剂。吸附剂的比表面积和平均孔径分别为79.5μm(2 )g(-1)和4.83nm。将蜂蜜样品在50℃下溶解在水(5%w / v)中10分钟,以4000rpm离心15分钟,最后在进行萃取之前使用滤纸过滤。研究了该方法的重要因素,以获得最佳条件。在最佳条件下(样品溶液,100mL;吸附剂,40mg; pH 5;提取时间,10分钟;解吸溶剂; MeOH,200 mu L),TC和CF检测限率为15.3和3.0μgkg (-1)。线性动态范围(LDR)得到10-5000μgkg(-1),分别为0.9939和0.9959的确定系数(R-2)。实际样品提取回收率分别为TC和CF的89-94%和95-98%。 TC的日期和日期的诊断为5.6和4.9%(n = 3),3.6和4.5%(n = 9)。

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