化学
固相萃取
检出限
吸附
萃取(化学)
色谱法
固相微萃取
二氧化钛
解吸
吸附剂
气相色谱-质谱法
质谱法
化学工程
有机化学
工程类
作者
Xiaohua Sun,Zhibo Fu,Tianyu Jiang,Fanghong Ning,Yongzhe Cheng,Tianhao Fu,Mingsheng Zhu,Hong-Fei Zhang,Ming Zhang,Ping Hu
标识
DOI:10.1016/j.chroma.2021.462750
摘要
• We had designed and prepared a hybrid nanocomposite material: β-Cyclodextrin MOF/TiO 2 . • This material was used as an adsorbent in D-SPE procedure for efficient adsorption of organochlorine pesticides. • D-SPE/GC–MS/MS were used for extraction and detection of organochlorine pesticides in honey water samples, which reduced the detection limit superiorly. • The strategy has good stability and repeatability, also has the characteristics of convenience and low cost. A simple and efficient dispersive solid-phase extraction (D-SPE) method combined with gas chromatography tandem mass spectrometry (GC-MS/MS) was developed to determine organochlorine pesticides (OCP) in honey. Firstly, a type of hybrid nanocomposite (CD-MOF/TiO 2 ) was prepared by grafting a metal-organic framework material synthesized with cyclodextrin as an organic ligand onto titanium dioxide. Then, the CD-MOF/TiO 2 was used as a D-SPE adsorbent to extract the OCP, and the effects of the amount of adsorbent, ultrasonic time, vortex time, pH, and salinity on the extraction were investigated using Plackett–Burman design and Box-Behnken Design. Under the optimized adsorption and desorption conditions, an analysis method that combined D-SPE with GC-MS/MS was established. The linear ranges of 14 OCP are 1–500 μg kg −1 and the correlation coefficients are between 0.9991 and 1.000. The limits of detection and quantification vary from 0.01 to 0.04 μg kg −1 and 0.04 to 0.12 μg kg −1 , respectively. The intra-day and inter-day precision of this method are suitable (RSDs% less than 11.3%). The established CD-MOF/TiO 2 / D-SPE method was used for the extraction of OCP in honey samples with recovery in the range of 76.4 to 114.3%. The results demonstrate that the CD-MOF/TiO 2 has a good selective enrichment ability for OCP and is suitable for the D-SPE pretreat of honey sample analysis.
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