Microwave-Assisted Synthesis of Magnetic Molecularly Imprinted Polymer Beads for The Rapid Determination of Diclofenac in Aqueous Samples Using HPLC-PAD

• Main Authors: Chieh-Yen Lee, 李婕晏
• Other Authors: Jen-Fon Jen
• Format: Others
• Language: zh-TW
• Published: 2012
• Online Access: http://ndltd.ncl.edu.tw/handle/09754671871696783524

碩士 === 國立中興大學 === 化學系所 === 100 === Diclofenac (DFC) is one of the most frequently used non-steroidal anti-inflammatory drugs with analgesic, antipyretic and anti-inflammatory effect. Due to its extensive use and bioaccumulation effect, DFC has been considered as one of the most commonly detected pharmaceutical residues in water bodies thus far. In order to realize the contamination level of DFC residues in the water sample, we have developed a rapid and sensitive sample preparation method using microwave (MW) assisted synthesized magnetic molecularly imprinted polymer (MMIP) beads as sorbents for dispersive solid phase microextaction (DSPME) coupled with HPLC-PAD analysis. The optimum conditions for MW assisted synthesized MMIP such as the ratio of reagents, microwave irradiation power and time, as well as the mircoextraction and chromatographic conditions were investigated. Under the optimal conditions, linear range was ranged from 0.1-50 μg.mL-1 with the correlation coefficient of 0.9953. Detection limit was 0.07 μg.mL-1. The MMIP-DSPME-HPLC/PAD method was applied to river water samples successfully and the relative recovery was ranged from 96.9-99.5 % with precision (RSD) of 1.5-4.3 % (n=3) when spiked with 0.25-25 μg.mL-1 of DFC in real water samples. The reproducibility of the MW assisted MMIP synthesis was 1.6 % for intra-batch (n=3) and 3.2 % for inter-batch (n=3). The result indicated that the MMIP obtained by the MW-assisted synthesis was with satisfactory reproducibility and high durability. The proposed MMIP-DSPME -HPLC/PAD method is a simple, rapid, selective, and cost-less method for the determination of DFC in water samples. Moreover, the proposed method reduces the interference of the substrate/water sample matrix and provides high selectivity. Thus, this method is proven to be an alternative method to analyze the DFC residue in the field of environmental water analysis in the future.