Jiyu Kim, Sumin Seo, Chohee Jeong, Eunbin Bae, Donghee Lee, Juhyeon Kim, Eunjin Ko, Hamin Choi, Sang Beom Han
{"title":"串联偶联色谱柱提高了 93 种芬太尼类似物的快速分离和预测性相互作用理解能力","authors":"Jiyu Kim, Sumin Seo, Chohee Jeong, Eunbin Bae, Donghee Lee, Juhyeon Kim, Eunjin Ko, Hamin Choi, Sang Beom Han","doi":"10.1016/j.aca.2024.343479","DOIUrl":null,"url":null,"abstract":"<div><h3>Background</h3><div>The simplicity of synthesis methods has facilitated the illegal manufacture of various fentanyl analogs, leading to numerous fatal overdoses worldwide, particularly in North America. Fentanyl analogs with similar structures are difficult to distinguish due to their fragmentation patterns, making separation using chromatography essential. Additionally, because fentanyl analogs are lethal even in trace amounts, they are easily smuggled, and commonly used fentanyl test strips often fail to detect them due to their low sensitivity. Therefore, the urgent need for analytical methods that can simultaneously identify multiple analogs and swiftly detect them at low concentrations.</div></div><div><h3>Results</h3><div>In this study, liquid chromatography-tandem mass spectrometry was conducted to screen 93 types of fentanyl analogs among the illegal fentanyl substances. The phenyl-hexyl columns enhance fentanyl analog separation through strong π–π interactions. The serially coupled column system increased the separation efficiency and mitigated peak distortion, particularly those of polar fentanyl analogs. The selectivity varied significantly, depending on the interactions with the combined columns. The phenyl-hexyl column's superior ability to predict fentanyl analog interactions based on molecular structure was confirmed by retention factor analysis. The resolution of fentanyl isomers increased significantly when methanol was used instead of acetonitrile as an organic modifier in the mobile phase. The approach was validated by determining the limits of detection and quantification, specificity, detection capability, recovery, and relative ion intensity.</div></div><div><h3>Significance</h3><div>The fentanyl analogs, including 23 sets of isomeric and isobaric compounds, were analyzed via separation using a phenyl-hexyl column serially coupled with a cyano column. The serially coupled column system increased the separation efficiency and mitigated peak distortion, particularly those of polar fentanyl analogs. The proposed strategy can be adopted in exploring methods of effectively separating mixtures with diverse properties, aiding the prevention of drug abuse and bolstering public health and safety efforts.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1336 ","pages":"Article 343479"},"PeriodicalIF":5.7000,"publicationDate":"2024-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Serially coupled columns enhance rapid separation and predictive interaction understanding of 93 fentanyl analogs\",\"authors\":\"Jiyu Kim, Sumin Seo, Chohee Jeong, Eunbin Bae, Donghee Lee, Juhyeon Kim, Eunjin Ko, Hamin Choi, Sang Beom Han\",\"doi\":\"10.1016/j.aca.2024.343479\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><h3>Background</h3><div>The simplicity of synthesis methods has facilitated the illegal manufacture of various fentanyl analogs, leading to numerous fatal overdoses worldwide, particularly in North America. Fentanyl analogs with similar structures are difficult to distinguish due to their fragmentation patterns, making separation using chromatography essential. Additionally, because fentanyl analogs are lethal even in trace amounts, they are easily smuggled, and commonly used fentanyl test strips often fail to detect them due to their low sensitivity. Therefore, the urgent need for analytical methods that can simultaneously identify multiple analogs and swiftly detect them at low concentrations.</div></div><div><h3>Results</h3><div>In this study, liquid chromatography-tandem mass spectrometry was conducted to screen 93 types of fentanyl analogs among the illegal fentanyl substances. The phenyl-hexyl columns enhance fentanyl analog separation through strong π–π interactions. The serially coupled column system increased the separation efficiency and mitigated peak distortion, particularly those of polar fentanyl analogs. The selectivity varied significantly, depending on the interactions with the combined columns. The phenyl-hexyl column's superior ability to predict fentanyl analog interactions based on molecular structure was confirmed by retention factor analysis. The resolution of fentanyl isomers increased significantly when methanol was used instead of acetonitrile as an organic modifier in the mobile phase. The approach was validated by determining the limits of detection and quantification, specificity, detection capability, recovery, and relative ion intensity.</div></div><div><h3>Significance</h3><div>The fentanyl analogs, including 23 sets of isomeric and isobaric compounds, were analyzed via separation using a phenyl-hexyl column serially coupled with a cyano column. The serially coupled column system increased the separation efficiency and mitigated peak distortion, particularly those of polar fentanyl analogs. The proposed strategy can be adopted in exploring methods of effectively separating mixtures with diverse properties, aiding the prevention of drug abuse and bolstering public health and safety efforts.</div></div>\",\"PeriodicalId\":240,\"journal\":{\"name\":\"Analytica Chimica Acta\",\"volume\":\"1336 \",\"pages\":\"Article 343479\"},\"PeriodicalIF\":5.7000,\"publicationDate\":\"2024-11-26\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Analytica Chimica Acta\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0003267024012807\",\"RegionNum\":2,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Analytica Chimica Acta","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0003267024012807","RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
Serially coupled columns enhance rapid separation and predictive interaction understanding of 93 fentanyl analogs
Background
The simplicity of synthesis methods has facilitated the illegal manufacture of various fentanyl analogs, leading to numerous fatal overdoses worldwide, particularly in North America. Fentanyl analogs with similar structures are difficult to distinguish due to their fragmentation patterns, making separation using chromatography essential. Additionally, because fentanyl analogs are lethal even in trace amounts, they are easily smuggled, and commonly used fentanyl test strips often fail to detect them due to their low sensitivity. Therefore, the urgent need for analytical methods that can simultaneously identify multiple analogs and swiftly detect them at low concentrations.
Results
In this study, liquid chromatography-tandem mass spectrometry was conducted to screen 93 types of fentanyl analogs among the illegal fentanyl substances. The phenyl-hexyl columns enhance fentanyl analog separation through strong π–π interactions. The serially coupled column system increased the separation efficiency and mitigated peak distortion, particularly those of polar fentanyl analogs. The selectivity varied significantly, depending on the interactions with the combined columns. The phenyl-hexyl column's superior ability to predict fentanyl analog interactions based on molecular structure was confirmed by retention factor analysis. The resolution of fentanyl isomers increased significantly when methanol was used instead of acetonitrile as an organic modifier in the mobile phase. The approach was validated by determining the limits of detection and quantification, specificity, detection capability, recovery, and relative ion intensity.
Significance
The fentanyl analogs, including 23 sets of isomeric and isobaric compounds, were analyzed via separation using a phenyl-hexyl column serially coupled with a cyano column. The serially coupled column system increased the separation efficiency and mitigated peak distortion, particularly those of polar fentanyl analogs. The proposed strategy can be adopted in exploring methods of effectively separating mixtures with diverse properties, aiding the prevention of drug abuse and bolstering public health and safety efforts.
期刊介绍:
Analytica Chimica Acta has an open access mirror journal Analytica Chimica Acta: X, sharing the same aims and scope, editorial team, submission system and rigorous peer review.
Analytica Chimica Acta provides a forum for the rapid publication of original research, and critical, comprehensive reviews dealing with all aspects of fundamental and applied modern analytical chemistry. The journal welcomes the submission of research papers which report studies concerning the development of new and significant analytical methodologies. In determining the suitability of submitted articles for publication, particular scrutiny will be placed on the degree of novelty and impact of the research and the extent to which it adds to the existing body of knowledge in analytical chemistry.