{"title":"开发一种柱上痕量富集方法,利用 RP-HPLC 和荧光检测法测定瓶装水中低于微克/升的双酚 A","authors":"Kevin C. Honeychurch","doi":"10.1155/2024/8258123","DOIUrl":null,"url":null,"abstract":"A simple extraction-free, on-column trace enrichment liquid chromatographic method for the determination of trace levels of bisphenol A (BPA) in bottled water samples has been developed. It was found possible to determine ng/L (ppt) levels of BPA by the direct introduction of 6 mL of sample water to the HPLC column utilising fluorescence detection (Ex<i>λ</i> = 274 nm, Em<i>λ</i> = 314 nm). Following the loading of the sample and the chromatographic focusing of the BPA on the analytical column, a simple switch from the aqueous sample to the isocratic chromatographic elution step of 50% acetonitrile/deionised water was undertaken. Using a BPA concentration of 0.596 <i>μ</i>g/L the effect of sample volume was investigated over the range 1.0 to 12 mL. A linear relationship with the sample volume introduced to the HPLC column and the resulting peak height for BPA was found over the entire range investigated <span><svg height=\"13.8595pt\" style=\"vertical-align:-2.2681pt\" version=\"1.1\" viewbox=\"-0.0498162 -11.5914 65.2093 13.8595\" width=\"65.2093pt\" xmlns=\"http://www.w3.org/2000/svg\" xmlns:xlink=\"http://www.w3.org/1999/xlink\"><g transform=\"matrix(.013,0,0,-0.013,0,0)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,4.498,0)\"></path></g><g transform=\"matrix(.0091,0,0,-0.0091,12.649,-5.741)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,21.228,0)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,32.49,0)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,38.73,0)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,41.694,0)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,47.936,0)\"><use xlink:href=\"#g113-58\"></use></g><g transform=\"matrix(.013,0,0,-0.013,54.177,0)\"><use xlink:href=\"#g113-58\"></use></g><g transform=\"matrix(.013,0,0,-0.013,60.418,0)\"></path></g></svg>.</span> Using a sample volume of 6.0 mL, a well-defined chromatographic peak was recorded for BPA over the concentration range of 0.1 <i>μ</i>g/L to 6.25 <i>μ</i>g/L <span><svg height=\"13.8595pt\" style=\"vertical-align:-2.2681pt\" version=\"1.1\" viewbox=\"-0.0498162 -11.5914 71.4727 13.8595\" width=\"71.4727pt\" xmlns=\"http://www.w3.org/2000/svg\" xmlns:xlink=\"http://www.w3.org/1999/xlink\"><g transform=\"matrix(.013,0,0,-0.013,0,0)\"><use xlink:href=\"#g113-41\"></use></g><g transform=\"matrix(.013,0,0,-0.013,4.498,0)\"><use xlink:href=\"#g113-83\"></use></g><g transform=\"matrix(.0091,0,0,-0.0091,12.649,-5.741)\"><use xlink:href=\"#g50-51\"></use></g><g transform=\"matrix(.013,0,0,-0.013,21.228,0)\"><use xlink:href=\"#g117-34\"></use></g><g transform=\"matrix(.013,0,0,-0.013,32.49,0)\"><use xlink:href=\"#g113-49\"></use></g><g transform=\"matrix(.013,0,0,-0.013,38.73,0)\"><use xlink:href=\"#g113-47\"></use></g><g transform=\"matrix(.013,0,0,-0.013,41.694,0)\"><use xlink:href=\"#g113-58\"></use></g><g transform=\"matrix(.013,0,0,-0.013,47.936,0)\"><use xlink:href=\"#g113-58\"></use></g><g transform=\"matrix(.013,0,0,-0.013,54.177,0)\"><use xlink:href=\"#g113-58\"></use></g><g transform=\"matrix(.013,0,0,-0.013,60.418,0)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,66.658,0)\"><use xlink:href=\"#g113-42\"></use></g></svg>.</span> A limit of detection of 0.058 <i>μ</i>g/L for BPA was calculated based on 3 <i>δ</i>. A mean recovery of 100% with an associated %CV of 7.6% (<i>n</i> = 5) was obtained for a bottled spring water sample fortified with 1.25 <i>μ</i>g/L BPA. Samples can be processed in under 12 minutes, much faster than that commonly reported for conventional offline extraction and chromatographic-based methods. The results show that the optimised method holds promise for the determination of BPA in such samples.","PeriodicalId":13888,"journal":{"name":"International Journal of Analytical Chemistry","volume":"187 3 1","pages":""},"PeriodicalIF":1.5000,"publicationDate":"2024-01-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Development of an On-Column Trace Enrichment Method for the Determination of Sub-μg/L Bisphenol A in Bottled Water by RP-HPLC with Fluorescent Detection\",\"authors\":\"Kevin C. 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引用次数: 0
摘要
我们开发了一种简单的免萃取柱上痕量富集液相色谱法,用于测定瓶装水样品中的双酚 A (BPA)痕量水平。该方法利用荧光检测(Exλ = 274 nm,Emλ = 314 nm),将 6 mL 样品水直接引入 HPLC 色谱柱,即可测定 ng/L (ppt) 级别的双酚 A。上样并在分析柱上对双酚 A 进行色谱聚焦后,从水样简单切换到 50% 乙腈/去离子水的等度色谱洗脱步骤。使用 0.596 μg/L 的双酚 A 浓度,在 1.0 至 12 mL 的范围内考察了样品量的影响。在整个研究范围内,双酚 A 与进入高效液相色谱柱的样品量和产生的峰高呈线性关系。使用 6.0 mL 的样品量,在 0.1 μg/L 至 6.25 μg/L 的浓度范围内,双酚 A 的色谱峰清晰可见。根据 3 δ 计算,双酚 A 的检测限为 0.058 μg/L。对于添加了 1.25 μg/L BPA 的瓶装矿泉水样品,平均回收率为 100%,相关的 %CV 为 7.6%(n = 5)。样品的处理时间不到 12 分钟,比传统的离线萃取和色谱法快得多。结果表明,优化后的方法有望测定此类样品中的双酚 A。
Development of an On-Column Trace Enrichment Method for the Determination of Sub-μg/L Bisphenol A in Bottled Water by RP-HPLC with Fluorescent Detection
A simple extraction-free, on-column trace enrichment liquid chromatographic method for the determination of trace levels of bisphenol A (BPA) in bottled water samples has been developed. It was found possible to determine ng/L (ppt) levels of BPA by the direct introduction of 6 mL of sample water to the HPLC column utilising fluorescence detection (Exλ = 274 nm, Emλ = 314 nm). Following the loading of the sample and the chromatographic focusing of the BPA on the analytical column, a simple switch from the aqueous sample to the isocratic chromatographic elution step of 50% acetonitrile/deionised water was undertaken. Using a BPA concentration of 0.596 μg/L the effect of sample volume was investigated over the range 1.0 to 12 mL. A linear relationship with the sample volume introduced to the HPLC column and the resulting peak height for BPA was found over the entire range investigated . Using a sample volume of 6.0 mL, a well-defined chromatographic peak was recorded for BPA over the concentration range of 0.1 μg/L to 6.25 μg/L . A limit of detection of 0.058 μg/L for BPA was calculated based on 3 δ. A mean recovery of 100% with an associated %CV of 7.6% (n = 5) was obtained for a bottled spring water sample fortified with 1.25 μg/L BPA. Samples can be processed in under 12 minutes, much faster than that commonly reported for conventional offline extraction and chromatographic-based methods. The results show that the optimised method holds promise for the determination of BPA in such samples.
期刊介绍:
International Journal of Analytical Chemistry publishes original research articles that report new experimental results and methods, especially in relation to important analytes, difficult matrices, and topical samples. Investigations may be fundamental, or else related to specific applications; examples being biological, environmental and food testing, and analysis in chemical synthesis and materials processing.
As well as original research, the International Journal of Analytical Chemistry also publishes focused review articles that examine the state of the art, identify emerging trends, and suggest future directions for developing fields.