Hannes Georg Graf, Thomas Ortmann, Peilin Yang, Edgar Naegele, Jingchun Yang, Shayne Green, Matthias Pursch
{"title":"克服强烈的样品溶剂效应,应对液相色谱法中的可持续性测量挑战。以双酚 A 为例","authors":"Hannes Georg Graf, Thomas Ortmann, Peilin Yang, Edgar Naegele, Jingchun Yang, Shayne Green, Matthias Pursch","doi":"10.1021/acs.analchem.4c03624","DOIUrl":null,"url":null,"abstract":"This paper describes an approach to achieve low parts per billion (ppb) concentration level detection using a reversed-phase ultrahigh-performance liquid chromatographic ultraviolet absorbance detection method with large-volume feed injection (FI) for analytes in dichloromethane (DCM). FI is a novel technology that allows sample injection at a defined speed into the LC mobile phase. We demonstrate this approach for a mixture of bisphenol A and its diglycidyl ether derivatives in DCM. DCM is a very strong injection solvent at reversed-phase LC conditions and is typically immiscible with a starting reversed-phase gradient mobile phase containing a high percentage of water. As a result, reduced separation performance and even peak splitting are seen with classic flow-through injection. The method setup comprised an octyl-bonded core–shell stationary phase (150 × 4.6 mm i.d., 2.7 μm particle size) with a water/acetonitrile mobile phase gradient and an exceptionally high injection volume of 45 μL of DCM solution using FI. Optimization of feed speed (1%) and isocratic hold duration (4 min) was crucial for final separation conditions. FI delivered more than a 20-fold improvement in the limit of detection (LOD) compared to standard flow-through injection while maintaining peak resolution. The LOD of the final method ranged between 1 and 10 ppb in the polymer resin. This methodology has high potential for trace analysis in a large variety of applications that suffer from the “strong solvent effect”.","PeriodicalId":27,"journal":{"name":"Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":6.7000,"publicationDate":"2024-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Overcoming the Strong Sample Solvent Effect for Sustainability Measurement Challenges in Liquid Chromatography. 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As a result, reduced separation performance and even peak splitting are seen with classic flow-through injection. The method setup comprised an octyl-bonded core–shell stationary phase (150 × 4.6 mm i.d., 2.7 μm particle size) with a water/acetonitrile mobile phase gradient and an exceptionally high injection volume of 45 μL of DCM solution using FI. Optimization of feed speed (1%) and isocratic hold duration (4 min) was crucial for final separation conditions. FI delivered more than a 20-fold improvement in the limit of detection (LOD) compared to standard flow-through injection while maintaining peak resolution. The LOD of the final method ranged between 1 and 10 ppb in the polymer resin. 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Overcoming the Strong Sample Solvent Effect for Sustainability Measurement Challenges in Liquid Chromatography. Example for Bisphenol-A
This paper describes an approach to achieve low parts per billion (ppb) concentration level detection using a reversed-phase ultrahigh-performance liquid chromatographic ultraviolet absorbance detection method with large-volume feed injection (FI) for analytes in dichloromethane (DCM). FI is a novel technology that allows sample injection at a defined speed into the LC mobile phase. We demonstrate this approach for a mixture of bisphenol A and its diglycidyl ether derivatives in DCM. DCM is a very strong injection solvent at reversed-phase LC conditions and is typically immiscible with a starting reversed-phase gradient mobile phase containing a high percentage of water. As a result, reduced separation performance and even peak splitting are seen with classic flow-through injection. The method setup comprised an octyl-bonded core–shell stationary phase (150 × 4.6 mm i.d., 2.7 μm particle size) with a water/acetonitrile mobile phase gradient and an exceptionally high injection volume of 45 μL of DCM solution using FI. Optimization of feed speed (1%) and isocratic hold duration (4 min) was crucial for final separation conditions. FI delivered more than a 20-fold improvement in the limit of detection (LOD) compared to standard flow-through injection while maintaining peak resolution. The LOD of the final method ranged between 1 and 10 ppb in the polymer resin. This methodology has high potential for trace analysis in a large variety of applications that suffer from the “strong solvent effect”.
期刊介绍:
Analytical Chemistry, a peer-reviewed research journal, focuses on disseminating new and original knowledge across all branches of analytical chemistry. Fundamental articles may explore general principles of chemical measurement science and need not directly address existing or potential analytical methodology. They can be entirely theoretical or report experimental results. Contributions may cover various phases of analytical operations, including sampling, bioanalysis, electrochemistry, mass spectrometry, microscale and nanoscale systems, environmental analysis, separations, spectroscopy, chemical reactions and selectivity, instrumentation, imaging, surface analysis, and data processing. Papers discussing known analytical methods should present a significant, original application of the method, a notable improvement, or results on an important analyte.