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LC Determination of Thiols Derivatized with 4-(Aminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole after SPE

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Abstract

Solid-phase extraction (SPE) coupled with high-performance liquid chromatography–fluorescence detection (LC–FL) was developed for the determination of three thiol compounds including glutathione, cysteine and acetylcysteine. 4-(Aminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole was used for derivatization of thiols. Factors affecting derivatization and extraction efficiency were optimized. Sample solution (2 mL) was extracted on a SPE column for 2 min and then eluted with 400 μL methanol. The analytes were injected onto the LC system for separation on a C18 column, and eluted with methanol–acetate buffer. The analytes were detected by fluorescence at an emission wavelength of 515 nm with excitation at 385 nm. The linearity of the method was in the range of 0.1–60 μM, with correlation coefficients ranging from 0.9979 to 0.9990. The detection limits of the method were in the range of 5–20 nM. The proposed method was applied to the analysis of human plasma samples with recoveries of 86–112.9%.

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Acknowledgments

This work was supported by the National Natural Science Foundation of China (20805040), Program for Science & Technology Innovation Talents in Universities of He’nan Province (2010HASTIT025), Excellent Youth Foundation of He’nan Scientific Committee (104100510020), and Research Foundation for Undergraduate of Xinyang Normal University (2010-DXS-70).

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Authors and Affiliations

  1. College of Chemistry and Chemical Engineering, Xinyang Normal University, Xinyang, 464000, China

    Ke-Jing Huang, Cong-Hui Han, Jing Li, Zhi-Wei Wu, Yan-Ming Liu & Ying-Ying Wu

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  1. Ke-Jing Huang
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  2. Cong-Hui Han
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  3. Jing Li
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Correspondence to Ke-Jing Huang.

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Huang, KJ., Han, CH., Li, J. et al. LC Determination of Thiols Derivatized with 4-(Aminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole after SPE. Chromatographia 74, 145–150 (2011). https://doi.org/10.1007/s10337-011-2025-3

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