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采用氰丙基功能化介孔硅 MCM-41 固相萃取,超高效液相色谱-串联质谱法测定水中的个人护理用品。

Determination of personal care products in water using UHPLC-MS after solid phase extraction with mesoporous silica-based MCM-41 functionalized with cyanopropyl groups.

机构信息

Department of Chemistry and Physics, Area of Analytical Chemistry, University of Almería, Almería, Spain.

Département de Chimie, Laboratoire de synthèse organique appliquée, Université Oran1, Oran, Algeria.

出版信息

J Sep Sci. 2020 Jun;43(11):2142-2153. doi: 10.1002/jssc.201901148. Epub 2020 Mar 13.

DOI:10.1002/jssc.201901148
PMID:32096598
Abstract

A silica-based MCM-41 mesoporous material functionalized with cyanopropyl groups has been synthesized by cocondensation, characterized and applied to preconcentrate six parabens and three UV filters in river and swimming-pool waters. The analytes were quantified by ultra-high performance liquid chromatography-tandem mass spectrometry, according to the Directive 96/23/EC. Even though matrix effect was negligible, quantification in river water samples with the standard addition approach improved the recoveries obtained using solvent-based and even with matrix-matched calibration. The method quantification limits in river water samples were 0.05 ng/mL for 2,4-dihydroxybenzophenone and 0.01 ng/mL for the rest. Recoveries, evaluated for a concentration level of 0.5 ng/L, were in the range 93.5-107.6% for parabens and in the range 64.2-85.8% for UV filters, with relative standard deviations intraday ≤10.2 and 10.8%, respectively. This parameter, evaluated for a concentration level of 0.1 ng/L, ranged between 98.3 and 110.4% for parabens and between 61.9 and 89.9% for UV filters, with relative standard deviation intraday ≤15.3 and 15.5%, respectively. The two UV filters with lower recoveries were the most affected by the addition of sodium chloride. River and swimming pool waters were analyzed and all the personal care products were found in the swimming pool water, whereas only methylparaben was detected in the river water.

摘要

一种基于硅胶的 MCM-41 介孔材料,通过共缩合反应功能化了氰丙基基团,已经被合成、表征,并应用于河流和游泳池水中六种对羟基苯甲酸酯和三种紫外线滤光剂的预浓缩。根据 96/23/EC 指令,采用超高效液相色谱-串联质谱法对分析物进行定量分析。尽管基质效应可以忽略不计,但采用标准添加法在河水样品中的定量,提高了基于溶剂的提取方法和甚至基质匹配校准的回收率。该方法在河水样品中的定量限为 0.05ng/mL 对 2,4-二羟基二苯甲酮和 0.01ng/mL 对其他物质。在 0.5ng/L 的浓度水平下,对羟基苯甲酸酯的回收率在 93.5-107.6%之间,紫外线滤光剂的回收率在 64.2-85.8%之间,日内相对标准偏差分别为≤10.2%和 10.8%。在 0.1ng/L 的浓度水平下,对羟基苯甲酸酯的回收率在 98.3-110.4%之间,紫外线滤光剂的回收率在 61.9-89.9%之间,日内相对标准偏差分别为≤15.3%和 15.5%。回收率较低的两种紫外线滤光剂受添加氯化钠的影响最大。对河流和游泳池水进行了分析,所有个人护理产品都在游泳池水中被发现,而在河水中只检测到了甲基对羟基苯甲酸酯。

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