固相萃取-超高效液相色谱-串联质谱法同时测定地表水中7种双酚类似物

Qiuxu Wang, Qiyan Feng, Guan-jiu Hu, Zhanqi Gao, Xueqiang Zhu, James Epua Epri
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引用次数: 14

摘要

为同时测定地表水中7种双酚类似物(bp),建立了固相萃取(SPE)与超高效液相色谱-串联质谱(UPLC-MS/MS)相结合的方法。通过优化固相萃取筒、pH、富集因子、流速、漂洗和洗脱体积等影响萃取效率的参数,提高了萃取效率。在单因素实验的基础上,尝试用响应面法获得优化结果,最佳参数为:以8 mL/min的流速,取1000ml水样通过亲水-亲脂平衡筒,用10%甲醇冲洗,用9ml甲醇洗脱,用自动固相萃取系统用氮气浓缩。色谱柱为Acquity UPLC BEH C18,流动相为乙腈- 0.05% (v/v)氨气,梯度洗脱,采用UPLC-MS/MS,负离子模式下多反应监测,色谱运行时间为8分钟。在1 ~ 500 μg/L范围内,7个bp具有良好的线性关系,相关系数均大于0.99。加样回收率为82.3% ~ 96.7%,基质效应为89.2% ~ 107%。结果表明,该方法回收率高,基质效应小。检出限为0.025 ~ 1.5 ng/L,相对标准偏差为2.9% ~ 8.5%。利用该方法,骆马湖共检测到5个bp,入流河流共检测到4个bp。BPA和BPF是主要的bp,其中BPA的浓度最高。结果表明,该方法灵敏、准确、高效,适用于地表水中7种bp的定性和定量分析。
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Simultaneous Determination of Seven Bisphenol Analogues in Surface Water by Solid-Phase Extraction and Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
For the simultaneous measurement of seven types of bisphenol analogues (BPs) in surface water, a method combining solid-phase extraction (SPE) with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The extraction efficiency was improved by optimizing the parameters that affect it, including the solid phase extraction cartridge, pH, enrichment factor, flow rate, rinsing and elution volumes. On the basis of a single factor experiment, an attempt to obtain the result of optimizing by response surface method was made, and the optimal parameters were as follows: at a flow rate of 8 mL/min, 1000 mL of water sample was run through the hydrophilic-lipophilic balancing cartridge, rinsed with 10% methanol, eluted with 9 mL methanol, and concentrated with nitrogen using an automatic solid-phase extraction system. The analytes were separated on an Acquity UPLC BEH C18 column using gradient elution with a mobile phase of acetonitrile and 0.05% (v/v) ammonia, and then analyzed using UPLC-MS/MS using multiple reaction monitoring in the negative-ion mode, with an 8-minute chromatographic run time. In the range of 1-500 μg/L, seven BPs showed good linearity with correlations greater than 0.99. The recovery ranged from 82.3%-96.7%, and the range of matrix effect was 89.2% to 107%. These results indicated excellent recovery and minimal matrix effect. The limits of detection were 0.025-1.5 ng/L, the relative standard deviation ranged were 2.9%-8.5%. Using the developed method, five BPs were detected in Luoma Lake and four BPs were detected in inflow rivers. BPA and BPF were the predominant BPs, and the concentration of BPA was the highest. The method was proved to be sensitive, accurate and efficient, and it was suitable for qualitative and quantitative analysis of seven BPs in surface water.
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