Department of Environmental Science, School of Tropical Medicine, International School of Public Health and One Health, Hainan Medical University, Haikou, 571199, China.
Laboratory of Pathogenic Biology and Immunology, School of Basic Medicine and Life Science, Hainan Medical University, Haikou, 571199, China.
Anal Chim Acta. 2023 Jun 22;1261:341225. doi: 10.1016/j.aca.2023.341225. Epub 2023 Apr 17.
A rapid, fast, widely applicable liquid-solid microextraction and purification method of triazine herbicides (TRZHs) in muti-media samples using salting-out assisted liquid-liquid extraction (SALLE) combined with self-assembled monolithic spin columns-solid phase micro extraction (MSC-SPME) was developed. Environmentally friendly coconut shell biochar (CSB) was used as the adsorbents of MSC-SPME. Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was the separation and determination method. The adsorption kinetics and isotherms were investigated to indicate the interaction between CSB and TRZHs. Several parameters influencing the liquid-solid microextraction efficiency, such as sample pH, salting-out solution volume and pH, sample loading speed, elution speed, elution ratio and volume of eluent were systematically investigated with the aid of orthogonal design. The whole extraction process was operated within 10 min. Under the optimum extraction and determination conditions, good linearities for three TRZHs were obtained in a range of 0.10-200.00 ng mL, with linear coefficients (R) greater than 0.999. The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 6.99-11.00 ng L and 23.33-36.68 ng L, respectively. The recoveries of the three TRZHs in multi-media environmental samples were ranged from 69.00% to 124.72%, with relative standard deviations (RSDs) lower than 0.43%. This SALLE-MSC-SPME-UPLC-MS/MS method was successfully applied to the determination of TRZHs in environmental and food samples and exhibited the advantages of high efficiency and sensitivity, low cost, and environmental friendliness. Compared with the methods published before, CSB-MSC was green, rapid, easy-operated, and reduced the whole cost of the experiment; SALLE combined MSC-SPME eliminated the matrix references effectively; what's more, the SALLE-MSC-SPME-UPLC-MS/MS method could be applied to various sample without complicated sample pretreatment procedure.
建立了一种快速、广泛适用于多介质样品中三嗪类除草剂(TRZHs)的盐析辅助液-液萃取(SALLE)与自组装整体柱-固相微萃取(MSC-SPME)相结合的液-固微萃取和净化方法。环境友好型椰子壳生物炭(CSB)被用作 MSC-SPME 的吸附剂。超高效液相色谱-串联质谱法(UPLC-MS/MS)为分离和测定方法。通过吸附动力学和等温线研究了 CSB 与 TRZHs 之间的相互作用。通过正交设计系统研究了影响液-固微萃取效率的几个参数,如样品 pH 值、盐析溶液体积和 pH 值、样品加载速度、洗脱速度、洗脱比和洗脱液体积。整个提取过程在 10 min 内完成。在最佳提取和测定条件下,三种 TRZHs 在 0.10-200.00ng mL 范围内均具有良好的线性,线性系数(R)大于 0.999。三种 TRZHs 的检出限(LODs)和定量限(LOQs)分别为 6.99-11.00 ng L 和 23.33-36.68 ng L。三种 TRZHs 在多介质环境样品中的回收率范围为 69.00%-124.72%,相对标准偏差(RSD)低于 0.43%。该 SALLE-MSC-SPME-UPLC-MS/MS 方法成功应用于环境和食品样品中 TRZHs 的测定,具有高效、灵敏、成本低、环境友好等优点。与以前发表的方法相比,CSB-MSC 绿色、快速、易于操作,降低了实验总成本;SALLE 结合 MSC-SPME 有效地消除了基质干扰;此外,SALLE-MSC-SPME-UPLC-MS/MS 方法可应用于各种无需复杂样品预处理程序的样品。