A rapid and inexpensive hydrothermal process was employed for the synthesis of a nanocomposite composed of zinc/aluminum-layered double hydroxide with carbonate interlayer anions and graphene oxide (Zn/Al LDH-GO). Fourier-transform infrared spectroscopy, scanning electron microscopy, Brunauer–Emmett–Teller area analysis, and X-ray diffraction technique were employed for the characterization of the prepared nanocomposite. Considering the possible cooperative adsorption effect of LDH and GO moieties, a column packed with this adsorbent has been used, for the first time, in the solid-phase extraction (SPE) of diclofenac. The analysis of DCF was carried out by employing high-performance liquid chromatography (HPLC). The parameters influencing the SPE and elution processes were optimized by the univariate sequential optimization procedure. Under optimized experimental conditions, the linear calibration plots for the determination of DCF in hospital wastewater and human serum samples were obtained in the ranges of 1–730 µg L⁻¹ (R² = 0.999) and 4–625 µg L⁻¹ (R² = 0.998), respectively. The limits of detections were correspondingly 0.12 and 0.5 µg L⁻¹, with the preconcentration factors of 68 and 59. The column stability was excellent, and its efficiency was almost constant, even after 192 adsorption/desorption cycles. The results confirmed the abilities of the developed method for the efficient preconcentration and thus precise trace analysis of DCF in real samples.

采用一种快速而廉价的水热法合成纳米复合材料，该复合材料由锌/铝层的双氢氧化物与碳酸盐夹层阴离子和氧化石墨烯（Zn / Al LDH-GO）组成。使用傅里叶变换红外光谱，扫描电子显微镜，Brunauer-Emmett-Teller面积分析和X射线衍射技术来表征所制备的纳米复合材料。考虑到LDH和GO部分可能的协同吸附作用，在双氯芬酸的固相萃取（SPE）中首次使用了装有该吸附剂的色谱柱。DCF的分析通过采用高效液相色谱法（HPLC）进行。通过单变量顺序优化程序优化了影响SPE和洗脱过程的参数。^-1（R ²  = 0.999）和4-625 µg L ^-1（R ²  = 0.998）。检测极限分别为0.12和0.5 µg L ^-1，预浓系数分别为68和59。即使经过192个吸附/解吸循环，色谱柱的稳定性也很出色，并且效率几乎恒定。结果证实了所开发的方法能够有效地进行预浓缩，从而对实际样品中的DCF进行精确的痕量分析。