使用 HPLC-DAD 方法同时测定地表水和废水基质中的 17 种酚类化合物

Iuliana Paun, Luoana Florentina Pascu, Vasile Ion Iancu, Florinela Pirvu, Toma Galaon, Florentina Laura Chiriac
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引用次数: 0

摘要

建立了一种高效液相色谱-二极管阵列检测器(HPLC-DAD)分析方法,用于同时检测两种水基质(废水和地表水)中的 17 种酚类化合物,包括酚、氯酚、烷基酚和硝基酚。在测定 HPLC-DAD 之前,对固相萃取 (SPE) 程序进行了优化。建议的方法采用多波长分析,最佳检测波长为 268 nm、280 nm、386 nm、304 nm 和 316 nm。色谱柱为 Eclipse XDB-C18(150 × 4.6 mm,5 μm),温度保持在 20 °C,分辨率最高。流动相采用梯度洗脱程序,流动相 A 为 0.1% H3PO4 水溶液,流动相 B 为乙腈。流速设定为 0.6 mL/min。17 种目标酚类化合物在不到 27 分钟的时间内完全分离。所有化合物的线性回归良好,相关系数均高于 0.999。该方法在地表水和废水中的定量限分别为 4.38 至 89.7 纳克/升和 7.83 至 167 纳克/升。地表水的回收率为 86.2-95.1%,废水的回收率为 79.1-86.3%。该方法快速、灵敏、准确、重现性好。所开发的方法被成功地应用于实际地表水和废水样品中 17 种酚类化合物的分析,其中苯酚、2,4-DNP 和 2,4-DNP 的测定值均高于方法的定量限(LOQ)。拟议的分析方法是同时测定环境水基质中 17 种酚类化合物的独创技术资源。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Simultaneous Determination of 17 Phenolic Compounds in Surface Water and Wastewater Matrices Using an HPLC-DAD Method
A high-performance liquid chromatography with diode array detector (HPLC-DAD) analytical method was developed for the simultaneous detection of 17 phenolic compounds, including phenols, chlorophenols, alkylphenols, and nitrophenols, in two types of water matrices: wastewater and surface water. Prior to HPLC-DAD determination, a solid-phase extraction (SPE) procedure was optimized. The proposed method uses multiwavelength analysis, with the optimum detection wavelengths selected as 268 nm, 280 nm, 386 nm, 304 nm, and 316 nm. The highest resolution was achieved using a chromatographic column, Eclipse XDB-C18 (150 × 4.6 mm, 5 μm), which was kept at 20 °C. The mobile phase consisted of a gradient elution program, with mobile phase A being a 0.1% H3PO4 aqueous solution and mobile phase B being acetonitrile. The flow rate was set at 0.6 mL/min. The 17 target phenolic compounds were fully separated in less than 27 min. All compounds showed good linear regression, with correlation coefficients higher than 0.999. The method’s quantitation limits ranged from 4.38 to 89.7 ng/L for surface water and 7.83 to 167 ng/L for wastewater. The recovery rates were in the range of 86.2–95.1% for surface water and 79.1–86.3% for wastewater. The SPE-HPLC-DAD method was proven to be fast, sensitive, accurate, and reproducible. The developed method was successfully applied for the analysis of the 17 phenolic compounds in real surface water and wastewater samples, with phenol, 2,4-DNP, and 2,4-DNP being determined at levels greater than the method’s limits of quantitation (LOQs). The proposed analytical method represents an original technical resource for the simultaneous determination of 17 phenolic compounds in environmental water matrices.
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