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基于交联羟丙基β-环糊精聚合物的分散固相萃取法用于同时测定水中三种手性三唑类杀菌剂对映体。

Dispersive solid phase extraction based on cross-linked hydroxypropyl β-cyclodextrin polymers for simultaneous enantiomeric determination of three chiral triazole fungicides in water.

作者信息

Zhang Chuhan, Tang Jing, Huang Yihe, Fan Ronghua, Zhou Li

机构信息

Department of Sanitary Inspection, School of Public Health, Shenyang Medical College, No. 146, North Huanghe Street, Liaoning Province, Shenyang, 110034, China.

School of Clinical Medicine, Beijing Tsinghua Changgung Hospital, Tsinghua University, Beijing, 102218, China.

出版信息

Mikrochim Acta. 2023 Dec 13;191(1):18. doi: 10.1007/s00604-023-06091-5.

DOI:10.1007/s00604-023-06091-5
PMID:38087124
Abstract

An efficient method is presented for simultaneous enantioselective determination of three chiral triazole fungicides (namely paclobutrazol, hexaconazole, and diniconazole) in water samples by DSPE-HPLC-UV. The perfect chiral separation of the enantiomers was achieved on a Chiralpak IH column within 15 min. In order to adsorb and enrich the analytes from water matrices, a cross-linked hydroxypropyl β-cyclodextrin polymer was synthesized. The prepared material exhibited good adsorption capacity, which was assessed by adsorption kinetic and adsorption thermodynamic experiments. One-variable-at-a-time and the response surface methodology were used to optimize the extraction parameters. Under the optimum sample preparation conditions, good linearity (2.0 ~ 800 µg L, R ≥ 0.9978), detection limits (0.6 to 1.0 µg L), quantitation limits (2.0 to 3.2 µg L), recoveries (86.7 ~ 105.8%), and the relative standard deviation (intra-day RSD ≤ 3.7%, inter-day RSD ≤ 5.1%) were obtained, satisfying the requirements of pesticides residues determination. These results demonstrated that the proposed method was applicable for routine determination of chiral triazole fungicide residues in water samples.

摘要

提出了一种通过分散固相萃取-高效液相色谱-紫外检测法同时对水样中三种手性三唑类杀菌剂(即多效唑、己唑醇和烯唑醇)进行对映体选择性测定的有效方法。在Chiralpak IH柱上15分钟内实现了对映体的完美手性分离。为了从水样中吸附和富集分析物,合成了一种交联羟丙基β-环糊精聚合物。通过吸附动力学和吸附热力学实验评估了所制备材料具有良好的吸附能力。采用单因素法和响应面法对萃取参数进行优化。在最佳样品制备条件下,获得了良好的线性关系(2.0~800μg/L,R≥0.9978)、检测限(0.6~1.0μg/L)、定量限(2.0~3.2μg/L)、回收率(86.7~105.8%)和相对标准偏差(日内RSD≤3.7%,日间RSD≤5.1%),满足农药残留测定的要求。这些结果表明,该方法适用于水样中手性三唑类杀菌剂残留的常规测定。

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