Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, P.O. Box 16315-1618, Tehran, Iran.
Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, P.O. Box 16315-1618, Tehran, Iran.
J Chromatogr A. 2020 Mar 15;1614:460718. doi: 10.1016/j.chroma.2019.460718. Epub 2019 Nov 18.
In the present work, NiFe layered double hydroxide (LDH)/Nylon 6 composite nanofibers were prepared by electrospinning method and used as a new sorbent for the extraction and measurement of non-steroidal anti-inflammatory drugs (naproxen, mefenamic acid, and diclofenac) in whole blood samples. The method is based on micro solid phase extraction (µSPE) by packed sorbent followed by HPLC-UV analysis. Effective parameters on the extraction efficiency were optimized using a central composite design (CCD). In order to characterize the sorbent, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), energy dispersive X-ray analysis (EDX) and elemental mapping were applied. The method was fully validated based on linearity, limits of detection (LOD) and quantification (LOQ), precision, and recovery. Under the optimal conditions, LOD values were found to be 25 ng mL for naproxen and diclofenac and 15 ng mL for mefenamic acid. A seven-point calibration curve was obtained in the range of 75-2000 ng mL for naproxen and diclofenac and 50-2000 for mefenamic acid. The method showed good linearity with coefficients of determination, r> 0.9962, for the three drugs. In the entire analytical range, the relative standard deviations (RSD%) were less than 8.1%. Finally, the efficiency of the method was investigated for the analysis of the target analytes in human blood samples, and the recoveries were obtained in the range of 90.7-109.8%.
在本工作中,通过静电纺丝法制备了 NiFe 层状双氢氧化物(LDH)/尼龙 6 复合纳米纤维,并将其用作提取和测量全血样品中非甾体抗炎药(萘普生、甲芬那酸和双氯芬酸)的新型吸附剂。该方法基于填充吸附剂的微固相萃取(µSPE),然后通过 HPLC-UV 分析。采用中心复合设计(CCD)优化了对萃取效率有影响的有效参数。为了对吸附剂进行表征,应用了傅里叶变换红外光谱(FTIR)、热重分析(TGA)、场发射扫描电子显微镜(FESEM)、能量色散 X 射线分析(EDX)和元素映射。该方法基于线性、检测限(LOD)和定量限(LOQ)、精密度和回收率进行了全面验证。在最佳条件下,萘普生和双氯芬酸的 LOD 值分别为 25 ng mL 和 15 ng mL,甲芬那酸的 LOD 值为 15 ng mL。萘普生和双氯芬酸的校准曲线在 75-2000 ng mL 范围内呈七点线性,甲芬那酸的校准曲线在 50-2000 ng mL 范围内呈七点线性。三种药物的相关系数,r>0.9962,均表现出良好的线性。在整个分析范围内,相对标准偏差(RSD%)小于 8.1%。最后,考察了该方法在人血样中分析目标分析物的效率,并获得了 90.7-109.8%的回收率。