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基于活性炭/硅藻土的磁性纳米复合材料用于从人尿中磁性固相萃取 S-苯巯基尿酸。

Activated carbon/diatomite-based magnetic nanocomposites for magnetic solid-phase extraction of S-phenylmercapturic acid from human urine.

机构信息

Hangzhou Occupational Disease Prevention and Control Hospital, Hangzhou, China.

China College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua, China.

出版信息

Biomed Chromatogr. 2020 Jul;34(7):e4834. doi: 10.1002/bmc.4834. Epub 2020 Apr 13.

Abstract

In this study, activated carbon/diatomite-based magnetic nancomposites (denoted as AC/DBMNs) were synthesized and applied as an adsorbent for magnetic solid-phase extraction of S-phenylmercapturic acid (S-PMA) from human urine prior to high-performance liquid chromatography. The surface morphologies and structures of AC/DBMNs were characterized by Fourier transform infrared spectroscopy, transmission and scanning electron microscopy, X-ray diffraction, Brunauer-Emmett-Teller surface area, vibrating sample magnetometer and ζ-potential measurements. The experimental parameters including sample volume, sample pH, adsorbent amount, extraction time, elution solvent and desorption time were investigated in detail. Under the optimum conditions, the method exhibited good linearity (r > 0.9993) within the concentration ranges of 0.03-1.0 mg/L. Moreover, the limits of detection and quantification were 0.01 and 0.03 mg/L, respectively. The enrichment factor was 5, and good recoveries (88.9-97.3%) with relative standard deviations in the range of 5.6-6.8% (n = 6) for inter-day and 6.3-8.1% (n = 6) for intra-day were achieved. The developed method was successfully applied to the analysis of S-PMA in urine samples. In addition, this accurate and sensitive method has great potential to be applied in the early screening and clinical diagnosis of the workers exposed to benzene.

摘要

在这项研究中,合成了基于活性炭/硅藻土的磁性纳米复合材料(表示为 AC/DBMNs),并将其用作高效液相色谱前从人尿中磁性固相萃取 S-苯巯基尿酸(S-PMA)的吸附剂。通过傅里叶变换红外光谱、透射电子显微镜和扫描电子显微镜、X 射线衍射、Brunauer-Emmett-Teller 表面积、振动样品磁强计和 ζ 电位测量对 AC/DBMNs 的表面形貌和结构进行了表征。详细研究了实验参数,包括样品体积、样品 pH 值、吸附剂用量、萃取时间、洗脱溶剂和洗脱时间。在最佳条件下,该方法在 0.03-1.0 mg/L 的浓度范围内表现出良好的线性(r > 0.9993)。此外,检测限和定量限分别为 0.01 和 0.03 mg/L。富集因子为 5,日内和日间相对标准偏差分别为 5.6-6.8%(n = 6)和 6.3-8.1%(n = 6)的回收率良好。该方法成功应用于尿液样品中 S-PMA 的分析。此外,该准确灵敏的方法具有很大的潜力,可用于接触苯的工人的早期筛查和临床诊断。

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