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辛基修饰的磁性石墨烯作为一种吸附剂,用于通过气相色谱-质谱联用技术萃取并同时测定水性样品中的香料过敏原、麝香和邻苯二甲酸酯。

Octyl-modified magnetic graphene as a sorbent for the extraction and simultaneous determination of fragrance allergens, musks, and phthalates in aqueous samples by gas chromatography with mass spectrometry.

作者信息

Maidatsi Katerina V, Chatzimitakos Theodoros G, Sakkas Vassilios A, Stalikas Constantine D

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina, Ioannina, Greece.

出版信息

J Sep Sci. 2015 Nov;38(21):3758-65. doi: 10.1002/jssc.201500578.

Abstract

An effective, simple, and low-cost sample preparation method based on dispersive SPE followed by GC with MS is developed for the multianalyte determination of fragrance allergens, musks, and phthalates, at sub-ppb levels. The extraction procedure is based on a novel magnetic graphene sorbent, which is functionalized with octylamine, taking advantage of the functionalization's hydrophobic properties and π-π interactions with the analytes. Two alkyl amines, the octylamine and octadecylamine are studied to introduce alkyl chains in the basal plane of graphene. Magnetic graphene- octadecylamine is proved to be highly hydrophobic to such a degree that is hard to disperse in the bulk aqueous matrixes. Because of this behavior, its extraction efficiency for the target analytes is low. The synthesis and applicability of the magnetic graphene-octylamine as more favored sorbent are optimized in terms of the most determining experimental conditions. The detection and quantification limits, which are calculated based on S/N ratio of 3 and 10, respectively, ranged from 0.29 to 3.2 ng L(-1) and from 0.89 to 9.6, respectively. The dispersive SPE is successfully applied to routine analysis for the determination of the target analytes in samples from municipal treatment plant of Ioannina (Greece), from Pamvotis Lake and baby bathwater. The reproducibility of the spiked biological treatment plant water sample is evaluated and the relative standard deviation values range between 2.1 and 9.4%.

摘要

开发了一种基于分散固相萃取(SPE),随后进行气相色谱-质谱联用(GC-MS)的有效、简单且低成本的样品制备方法,用于测定痕量水平的香料过敏原、麝香和邻苯二甲酸盐。萃取过程基于一种新型磁性石墨烯吸附剂,该吸附剂用辛胺进行了功能化处理,利用了功能化的疏水特性以及与分析物的π-π相互作用。研究了两种烷基胺,即辛胺和十八烷基胺,以在石墨烯的基面引入烷基链。事实证明,磁性石墨烯-十八烷基胺疏水性极强,以至于难以分散在大量水相中。由于这种特性,其对目标分析物的萃取效率较低。在最关键的实验条件方面,对作为更优吸附剂的磁性石墨烯-辛胺的合成及适用性进行了优化。基于信噪比分别为3和10计算得出的检测限和定量限分别为0.29至3.2 ng L⁻¹和0.89至9.6。分散固相萃取成功应用于常规分析,用于测定来自希腊约阿尼纳市污水处理厂、潘沃蒂斯湖和婴儿洗澡水样品中的目标分析物。对加标生物处理厂水样的重现性进行了评估,相对标准偏差值在2.1%至9.4%之间。

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