Institute of Environmental and Analysis Science, Center for Multi-Omic Research, School of Chemistry and Chemical Engineering, Henan University, Kaifeng, 475004, Henan, China.
State Key Laboratory of Environmental and Biological Analysis, Department of Chemistry, Hong Kong Baptist University, Hong Kong, 999077, China.
Mikrochim Acta. 2019 Apr 11;186(5):279. doi: 10.1007/s00604-019-3394-9.
Mesoporous graphitic carbon nitride (MCN) is shown to be a viable sorbent for the enrichment of sulfonamides (SAs). To overcome the difficulty of separating the sorbent from the matrix, a novel type kind of column-assisted dispersive solid-phase extraction (CA-dSPE) method was designed. The MCN was characterized by scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, fourier transform infrared spectroscopy and nitrogen adsorption-desorption measurements. The amount of sorbent, the pH value of the sample, the adsorption time, type and volume of the eluent and desorption time were optimized. The SAs were eluted from the sorbent with elution solvent of methanol containing 10% (v/v) ammonia and then submitted to HPLC analysis. Under the optimized conditions, the limits of detection for the SAs investigated (sulfadiazine, sulfameter, sulfachloropyridazine, sulfabenzamide and sulfadimethoxine) range from 20 to 5 pg·mL. Satisfactory recoveries were obtained for spiked environmental water (90.1-110.5%) and milk samples (82.3-102.7%), with relative standard deviations of 0.5-3.8% and 1.1-4.4%, respectively. The method is simple, time saving and sensitive. Graphical abstract Schematic presentation of a column assisted dispersive solid-phase extraction by using mesoporous graphitic carbon nitride as sorbent combined with high performance liquid chromatography for sensitive analysis of sulfonamides in environmental water and milk samples.
介孔石墨相氮化碳（MCN）被证明是一种可行的磺胺类药物（SAs）富集的吸附剂。为了克服从基质中分离吸附剂的困难，设计了一种新型的柱辅助分散固相萃取（CA-dSPE）方法。通过扫描电子显微镜、高分辨率透射电子显微镜、X 射线衍射、傅里叶变换红外光谱和氮气吸附-解吸测量对 MCN 进行了表征。优化了吸附剂的用量、样品的 pH 值、吸附时间、洗脱剂的类型和体积以及解吸时间。用含有 10%（v/v）氨的甲醇洗脱剂从吸附剂上洗脱磺胺类药物，然后进行 HPLC 分析。在优化的条件下，所研究的磺胺类药物（磺胺嘧啶、磺胺甲恶唑、磺胺氯哒嗪、磺胺苯甲酰胺和磺胺二甲氧嘧啶）的检出限范围为 20-5 pg·mL。环境水样（90.1-110.5%）和牛奶样品（82.3-102.7%）的加标回收率令人满意，相对标准偏差分别为 0.5-3.8%和 1.1-4.4%。该方法简单、省时、灵敏。
