Li Bingzhi, Chen Min, Li Yang, Cao Xiaolin, She Yongxin, Yin Jungang, Cong Shuang, Zhang Ziping
College of Life Science, Yantai University, Yantai, P. R. China.
Yantai Academy of Agricultural Sciences, Yantai, P. R. China.
J Sep Sci. 2022 Feb;45(3):752-759. doi: 10.1002/jssc.202100788. Epub 2021 Dec 16.
In this paper, a flower-like molybdenum disulfide material was prepared by hydrothermal method and was first used as adsorbents in the solid-phase extraction process for enriching N-nitrosoamines. Molybdenum disulfide exhibited three-dimensional petal-like microspheres with about 500 nm in diameter. The relevant analyte extraction and elution parameters (sample volumes, solution pH, washing solvents, elution solvents, and elution volumes) were optimized to improve the solid-phase extraction efficiency. The solid-phase extraction process coupled with high-performance liquid chromatography-tandem mass spectrometry for determining N-nitrosoamines in environmental water samples was established. The limits of detection were in the range of 0.01-0.05 ng/mL. The satisfactory recoveries (68.9-106.1%) were obtained at three different spiked concentrations (2, 5, and 8 ng/mL) in water samples, and the relative standard deviations were between 1.96 and 8.38%. This proposed method not only showed high sensitivity and good reusability but also provided a new adsorbent for enriching trace N-nitrosoamines in environmental water samples.
本文采用水热法制备了一种花状二硫化钼材料，并首次将其用作吸附剂用于固相萃取过程中富集N-亚硝胺。二硫化钼呈现出直径约500 nm的三维花瓣状微球。对相关的分析物萃取和洗脱参数（样品体积、溶液pH值、洗涤溶剂、洗脱溶剂和洗脱体积）进行了优化，以提高固相萃取效率。建立了固相萃取结合高效液相色谱-串联质谱法测定环境水样中N-亚硝胺的方法。检测限在0.01 - 0.05 ng/mL范围内。在水样的三个不同加标浓度（2、5和8 ng/mL）下获得了令人满意的回收率（68.9 - 106.1%），相对标准偏差在1.96%至8.38%之间。该方法不仅具有高灵敏度和良好的可重复使用性，还为富集环境水样中的痕量N-亚硝胺提供了一种新型吸附剂。
