Dummy molecularly imprinted microspheres prepared by Pickering emulsion polymerization for matrix solid-phase dispersion extraction of three azole fungicides from fish samples
Dummy molecularly imprinted microspheres prepared by Pickering emulsion polymerization for matrix solid-phase dispersion extraction of three azole fungicides from fish samples
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Pickering乳液聚合制备虚拟分子印迹微球用于基质固相分散萃取鱼样中的三种唑类杀菌剂
DOI：
10.1016/j.chroma.2020.461013
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发表时间：
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影响因子：
4.1
通讯作者：
Qinghua Zhou
中科院分区：
文献类型：
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作者：
Xinxue Zhang;Xiaoli Sun;Muhua Wang;Yan Wang;Qinyao Wu;Lv Ji;Qi Li;Jiajia Yang;Qinghua Zhou
采用Pickering乳液聚合法合成了虚拟分子印迹微球（DMIMs），并将其作为基质固相分散萃取（MSPD）吸附剂用于鱼样品中唑类杀菌剂的样品前处理。以α-（2，4-二氯苯基）-1H-咪唑-1-乙醇（DCE）为模板分子，对氯咪巴唑（CBZ）、克霉唑（CMZ）和咪康唑（MNZ）进行分子印迹。用扫描电镜（SEM）和氮气吸附法对微球的形貌进行了表征，微球粒径分布窄（20-50 μm），球形规则，比表面积高（SBET= 408.91 ± 6.72 m2 g-1）。静态吸附实验表明，DMIMs对CBZ、CMZ和MNZ具有良好的类选择性。以MSPD为吸附剂，对鱼样品中的CBZ、CMZ和MNZ进行了提取和纯化研究。采用HPLC-DAD检测器在225 nm处对提取的唑类杀菌剂进行检测。对MSPD的洗脱条件、样品/吸附剂质量比和洗涤条件进行了考察。对0.5、2.5和12.5 μg g g-1的鱼肉样品，该方法具有良好的回收率（89.2-101.5%）和重现性（RSD 1.6- 4.8%，n = 5）。CBZ、CMZ和MNZ的检出限分别为0.045、0.036和0.033 μg/g。结果表明，该方法对于鱼类样品中唑类杀菌剂的前处理具有良好的应用前景。
Dummy molecularly imprinted microspheres (DMIMs) were synthesized by Pickering emulsion polymerization and used as the matrix solid-phase dispersion extraction (MSPD) sorbent for sample pre-treatment of azole fungicides in fish samples. Alpha-(2,4-Dichlorophenyl)-1H-imidazole-1-ethanol (DCE) was used as the fragment dummy template for the imprinting of climbazole (CBZ), clotrimazole (CMZ) and miconazole (MNZ). The morphology of the microspheres were characterized by scanning electron microscopy (SEM) and nitrogen adsorption measurements, narrow diameter distribution (20–50 μm) with regular spherical shape and high surface area (SBET= 408.91 ± 6.72 m2g–1) were achieved. Good class-selectivity of the DMIMs was found for CBZ, CMZ and MNZ by static adsorption experiments. The imprinted microspheres as MSPD sorbent was then evaluated for the extraction and purification of CBZ, CMZ and MNZ in fish samples. The extracted azole fungicides were detected by HPLC-DAD analysis at 225 nm. MSPD conditions including elution, mass ratio of sample/sorbent and washing were carefully evaluated. The optimized MSPD method have good recoveries (89.2–101.5%) and reproducibility (RSDs 1.6–4.8%,n= 5) for fish samples spiked at 0.5, 2.5 and 12.5 μg g–1. The limits of detection (LODs) were 0.045, 0.036 and 0.033 μg g–1for CBZ, CMZ and MNZ, respectively. The results show that this method has a good application prospect for the pretreatment of azole fungicides in fish samples.