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响应面法优化同时检测土壤中磺胺甲恶唑和 17β-雌二醇的提取方法

Response Surface Optimization of an Extraction Method for the Simultaneous Detection of Sulfamethoxazole and 17β-Estradiol in Soil.

机构信息

School of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai 200240, China.

School of Chemistry and Chemical Engineering, Shanghai University of Engineering Science, Shanghai 201620, China.

出版信息

Molecules. 2020 Mar 20;25(6):1415. doi: 10.3390/molecules25061415.

Abstract

Antibiotics and hormones widely exist in fertilizers and manures, which are excessively used in agriculture and animal husbandry. Considering their potential harm to the environment and human health, the detection of antibiotics and hormones has become a necessity. However, current methods find it difficult to simultaneously extract and detect antibiotics and hormones in soil and to maintain a high level of accuracy and a low cost. In this study, a straightforward, convenient, and simultaneous extraction and detection method of a representative antibiotic (sulfamethoxazole, SMZ) and hormone (17β-Estradiol, E2) in soil has been established. Ultrasound-assisted extraction (UAE) was used in the pretreatment process and high-performance liquid chromatography with the ultraviolet detector (HPLC-UV) method was then chosen in the detection process. By means of single factors and response surface experiments, optimal extraction conditions were a 41-mL buffer solution (pH 4.27) mixed with 1 g of soil sample, an ultrasonication time of 36 min, an ultrasonication temperature of 25 °C, and two extraction cycles. The detection limits of 0.3-10 μg/kg and quantification limits of 1-30 μg/kg have been obtained. Finally, the optimized simultaneous extraction and detection method was validated by three different real soil samples with recoveries ranging from 79.49% to 86.47%.

摘要

抗生素和激素广泛存在于肥料和粪便中,这些在农业和畜牧业中被过度使用。考虑到它们对环境和人类健康的潜在危害,对抗生素和激素的检测已经成为必要。然而,目前的方法很难同时提取和检测土壤中的抗生素和激素,并且难以保持高精度和低成本。在这项研究中,建立了一种简单、方便且同时提取和检测土壤中代表性抗生素(磺胺甲恶唑,SMZ)和激素(17β-雌二醇,E2)的方法。在预处理过程中使用超声辅助提取(UAE),然后在检测过程中选择高效液相色谱与紫外检测器(HPLC-UV)法。通过单因素和响应面实验,获得了最佳的提取条件为:41 mL 缓冲溶液(pH 4.27)与 1 g 土壤样品混合,超声时间 36 min,超声温度 25°C,提取循环两次。检测限为 0.3-10 μg/kg,定量限为 1-30 μg/kg。最后,通过三种不同的实际土壤样品验证了优化的同时提取和检测方法,回收率在 79.49%至 86.47%之间。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3776/7144367/341013f6fd3a/molecules-25-01415-g001.jpg

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