State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, China.
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, China.
Talanta. 2018 Jul 1;184:411-417. doi: 10.1016/j.talanta.2018.03.005. Epub 2018 Mar 7.
In this work, a convenient and sensitive method for the determination of triazoles in environmental waters was developed by on-line combining in-tube solid phase microextraction (IT-SPME) and high performance liquid chromatography with diode array detector (HPLC-DAD). To extract triazoles effectively, poly (4-vinyl pyridine-co-ethylene dimethacrylate) monolith was in-situ fabricated and utilized as the extraction phase of IT-SPME. A series of key extraction parameters including desorption solvent, sample volume, adsorption and desorption flow rate, pH value and ionic strength in sample matrix were optimized thoroughly. Under the most favorable conditions (volume of sample, 6.0 mL; adsorption flow rate, 0.2 mL/min; desorption solvent, 80.0 µL mixture of ACN/water (70/30, v/v); desorption flow rate, 50.0 µL/min; sample pH value, 8.0; ionic strength did not be adjusted), the developed monolith-based IT-SPME could extract target analytes effectively and expected analytical merits were achieved. The limits of detection (S/N = 3) and limits of quantification (S/N = 10) were in the ranges of 0.014-0.031 µg/L and 0.11-0.074 µg/L, respectively. Satisfactory method reproducibility was obtained by intra-day and inter-day precisions, with relative standard deviations (RSDs) lower than 10%. The optimized IT-SPME-HPLC-DAD method was then applied to detect triadimenol, triazolone and hexaconazole in water samples including lake, river and sewage waters. The spiked recoveries were 78.9-106% and the RSDs were in the range of 0.2-7.2%. The results well evidence that the proposed method is convenient, accurate, sensitive, practical and environmentally friendly for the determination of triazoles in environmental waters.
在这项工作中，通过在线结合管内固相微萃取（IT-SPME）和高效液相色谱与二极管阵列检测器（HPLC-DAD），开发了一种用于测定环境水中三唑类化合物的方便、灵敏的方法。为了有效地萃取三唑类化合物，原位制备了聚（4-乙烯基吡啶-co-乙二醇二甲基丙烯酸酯）整体柱作为 IT-SPME 的萃取相。通过实验优化了一系列关键的萃取参数，包括解吸溶剂、样品体积、吸附和洗脱流速、样品基质中的 pH 值和离子强度。在最有利的条件下（样品体积为 6.0mL；吸附流速为 0.2mL/min；解吸溶剂为 80.0µL ACN/水（70/30，v/v）混合物；解吸流速为 50.0µL/min；样品 pH 值为 8.0；不调节离子强度），所开发的基于整体柱的 IT-SPME 可以有效地萃取目标分析物，并获得预期的分析性能。检测限（S/N=3）和定量限（S/N=10）的范围分别为 0.014-0.031µg/L 和 0.11-0.074µg/L。日内和日间精密度均获得了令人满意的方法重现性，相对标准偏差（RSD）低于 10%。然后将优化后的 IT-SPME-HPLC-DAD 方法应用于检测湖泊、河流和污水等水样中的三唑醇、三唑酮和己唑醇。加标回收率为 78.9-106%，RSD 范围为 0.2-7.2%。结果表明，该方法简便、准确、灵敏、实用、对环境水样中三唑类化合物的测定具有环保性。
