当前位置: X-MOL 学术Microchim. Acta › 论文详情
Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)
Graphitic carbon nitride as sorbent for the emulsification-enhanced disposable pipette extraction of eight organochlorine pesticides prior to GC-MS analysis
Microchimica Acta ( IF 5.7 ) Pub Date : 2020-01-14 , DOI: 10.1007/s00604-019-4107-0
Sze Chieh Tan 1, 2 , Hian Kee Lee 1, 2
Affiliation  

Graphitic carbon nitride (g-C 3 N 4 ) was explored as a sorbent for the emulsification-enhanced (EE) disposable pipette extraction (DPX) of eight organochlorine pesticides (OCPs) from environmental waters. The OCPs, including α-hexachlorocyclohexane, Aldrin, α-Chlordane, Dieldrin, 4,4′-dichlorodiphenyldichloroethylene, 4,4′-dichlorodiphenyldichloroethane, Heptachlor and Heptachlor epoxide (Isomer A), were analyzed by gas chromatography-mass spectrometry. The sorbent g-C 3 N 4 was characterized by elemental analysis, X-ray diffraction, scanning electron microscopy, Fourier-transform infrared and Raman spectroscopy. As a C-N analogue of graphite, g-C 3 N 4 exhibits good water dispersibility and allows easy analyte recovery – a characteristic not commonly observed in carbon-based materials. When applied to DPX, g-C 3 N 4 rapidly establishes strong interactions with the OCPs. Consequently, g-C 3 N 4 displays superior extraction capability in comparison to six other commercial sorbents. An emulsification step prior to DPX was found to enhance the overall extraction efficiency by pre-concentrating the OCPs into the microdroplets of an organic solvent. The microdroplets were then adsorbed onto g-C 3 N 4 . Under the most favorable conditions, wide linear responses spanning over two to four orders of magnitudes are established. The limits of detection range between 2.4 ng·L −1 and 46.2 ng·L −1 . The method is reproducible (relative standard deviations ≤ 7.4%) and enrichment factors are between 42 and 57. When applied to the analysis of lake and river water samples, EE-DPX-gas chromatography-mass spectrometry exhibits good resilience against matrix interferences. The relative recoveries range between 77.7% and 106.3%. In comparison to other sorbent-based extraction techniques reported for the analysis of OCPs in aqueous samples, EE-DPX utilizes the minimal amount of sample and solvent, and requires the shortest sample preparation time. Graphical abstract Schematic representation of the emulsification-enhanced disposable pipette extraction (DPX) of organochlorine pesticides (OCPs) using graphitic carbon nitride (g-C 3 N 4 ) as sorbent. Emulsification and DPX work synergistically, thus allowing rapid dissolution of analytes into microdroplets of organic solvent, before being extracted by g-C 3 N 4 .

中文翻译:

石墨氮化碳作为吸附剂,在 GC-MS 分析前对八种有机氯农药进行乳化增强的一次性移液管萃取

石墨氮化碳 (gC 3 N 4 ) 被探索作为一种吸附剂,用于从环境水中的八种有机氯农药 (OCP) 的乳化增强 (EE) 一次性移液器萃取 (DPX)。通过气相色谱-质谱法分析了 OCP,包括 α-六氯环己烷、艾氏剂、α-氯丹、狄氏剂、4,4'-二氯二苯基二氯乙烯、4,4'-二氯二苯基二氯乙烷、七氯和七氯环氧化物(异构体 A)。吸附剂 gC 3 N 4 通过元素分析、X 射线衍射、扫描电子显微镜、傅里叶变换红外光谱和拉曼光谱表征。作为石墨的 CN 类似物,gC 3 N 4 具有良好的水分散性,并且可以轻松回收分析物——这是碳基材料中不常见的特征。当应用于 DPX 时,gC 3 N 4 迅速与OCPs 建立强相互作用。因此,与其他六种商业吸附剂相比,gC 3 N 4 显示出卓越的萃取能力。发现在 DPX 之前的乳化步骤通过将 OCP 预浓缩到有机溶剂的微滴中来提高整体提取效率。然后将微滴吸附到gC 3 N 4 上。在最有利的条件下,可以建立跨越两到四个数量级的宽线性响应。检测范围在2.4 ng·L -1 和46.2 ng·L -1 之间。该方法重现性好(相对标准偏差≤7.4%),富集因子在42-57之间。应用于湖泊和河流水样分析时,EE-DPX-气相色谱-质谱具有良好的抗基质干扰能力。相对回收率介于 77.7% 和 106.3% 之间。与用于分析水性样品中 OCP 的其他基于吸附剂的萃取技术相比,EE-DPX 使用最少的样品和溶剂,并且需要最短的样品制备时间。图形摘要 使用石墨氮化碳 (gC 3 N 4 ) 作为吸附剂对有机氯农药 (OCP) 进行乳化增强的一次性移液管萃取 (DPX) 的示意图。乳化和 DPX 协同工作,从而使分析物在被 gC 3 N 4 萃取之前快速溶解到有机溶剂的微滴中。与用于分析水性样品中 OCP 的其他基于吸附剂的萃取技术相比,EE-DPX 使用最少的样品和溶剂,并且需要最短的样品制备时间。图形摘要 使用石墨氮化碳 (gC 3 N 4 ) 作为吸附剂对有机氯农药 (OCP) 进行乳化增强的一次性移液管萃取 (DPX) 的示意图。乳化和 DPX 协同工作,从而使分析物在被 gC 3 N 4 萃取之前快速溶解到有机溶剂的微滴中。与用于分析水性样品中 OCP 的其他基于吸附剂的萃取技术相比,EE-DPX 使用最少的样品和溶剂,并且需要最短的样品制备时间。图形摘要 使用石墨氮化碳 (gC 3 N 4 ) 作为吸附剂对有机氯农药 (OCP) 进行乳化增强的一次性移液管萃取 (DPX) 的示意图。乳化和 DPX 协同工作,从而使分析物在被 gC 3 N 4 萃取之前快速溶解到有机溶剂的微滴中。图形摘要 使用石墨氮化碳 (gC 3 N 4 ) 作为吸附剂对有机氯农药 (OCP) 进行乳化增强的一次性移液管萃取 (DPX) 的示意图。乳化和 DPX 协同工作,从而使分析物在被 gC 3 N 4 萃取之前快速溶解到有机溶剂的微滴中。图形摘要 使用石墨氮化碳 (gC 3 N 4 ) 作为吸附剂对有机氯农药 (OCP) 进行乳化增强的一次性移液管萃取 (DPX) 的示意图。乳化和 DPX 协同工作,从而使分析物在被 gC 3 N 4 萃取之前快速溶解到有机溶剂的微滴中。
更新日期:2020-01-14
down
wechat
bug