利用 pH 值可切换的深共晶溶剂和高效液相色谱-二极管阵列检测器建立运动营养品和健美补充剂中 1,3-二甲基胺的分析方法

IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Journal of separation science Pub Date : 2024-08-31 DOI:10.1002/jssc.202400340
Dijun Shen, Jie Zhang, Ying Zhang, Xiru Du
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引用次数: 0

摘要

本研究开发了一种基于液相微萃取的液相微萃取-高效液相色谱-二极管阵列检测器分析法,用于测定1,3-二甲基胺(DMAA)。通过改变 pH 值考察了所获得的 DES 的可切换性。然后对选出的最佳DES进行了表征,并研究了所选DES在从运动营养品和健美补充剂中提取DMAA中的应用。由 l-薄荷醇:油酸以 1:2 的摩尔比合成的 DES 对目标化合物的萃取效率最高。在最佳条件下(50 µL DES、100 µL 4 mol/L KOH、100 µL 4 mol/L HCl、萃取时间40 s且不加盐),校准图在0.05-100 µg/kg 范围内呈线性关系,检出限为0.02 µg/kg。实际样品中 10.0 µg/kg DMAA 的日内和日间相对标准偏差分别为 2.7% (n = 7) 和 5.3% (n = 7)。该方法的富集因子和提取回收率分别为 283% 和 85%。不同样品中 DMAA 的相对回收率在 90%-109% 之间。
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Development of analytical method for determination of 1,3-dimethylamylamine in sports nutrition and bodybuilding supplements using pH-switchable deep eutectic solvents followed by high-performance liquid chromatography-diode array detector

In this work, an easy, safe, simple, and efficient pH-switchable deep eutectic solvents (DESs)-based liquid phase microextraction followed by high-performance liquid chromatography-diode array detector analysis was developed for the determination of 1,3-dimethylamylamine (DMAA). The switchability of the obtained DESs was investigated by changing the pH. Then the best-selected DES was characterized and the application of the selected DES in the extraction of DMAA from sports nutrition and bodybuilding supplements was investigated. The DES synthesized from l-menthol: oleic acid in a molar ratio of 1:2 had the highest efficiency in the extraction of the target compound. Under the optimum conditions, (50 µL of DES, 100 µL of 4 mol/L KOH, 100 µL of 4 mol/L HCl, extraction time of 40 s and without salt addition) the calibration graph was linear in the range of 0.05–100 µg/kg and limit of detection was 0.02 µg/kg. The relative standard deviations including intra-day and inter-day for 10.0 µg/kg of DMAA in real samples were 2.7% (n = 7) and 5.3% (n = 7), respectively. The enrichment factor and percentage extraction recovery of the method were 283 and 85%, respectively. The relative recoveries for DMAA in different samples were in the range of 90%–109%.

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来源期刊
Journal of separation science
Journal of separation science 化学-分析化学
CiteScore
6.30
自引率
16.10%
发文量
408
审稿时长
1.8 months
期刊介绍: The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.
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