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Simultaneous determination of six alkaloids in blood and urine using a hydrophilic interaction liquid chromatography method coupled with electrospray ionization tandem mass spectrometry

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Abstract

A method was developed for the simultaneous determination of six toxic alkaloids (aconitine, hypaconitine, gelsemine, raceanisodamine, strychnine, brucine) in blood and urine by hydrophilic interaction liquid chromatography (HILIC) coupled with electrospray tandem mass spectrometry. Ephedrine was selected as the internal standard. Samples were extracted and cleaned up by solid-phase extraction (SPE) using Oasis MCX cartridges. Separation parameters such as organic modifier, buffer pH, and concentration of buffer salt were investigated. Gradient separation and analysis were achieved for six alkaloids on a 3-μm Atlantis HILIC column using a mobile phase consisting of 30 mM ammonium formate and acetonitrile at pH 3. Two multiple reaction monitoring (MRM) transitions for each substance were monitored to provide sufficient identification of alkaloid. The retention mechanisms were explored in the method development. Validation included assessment of linearity, limit of quantification, accuracy, and precision. Bias was less than 15.1% and precision was better than 8.3% for both blood and urine samples. A total of 54 clinical samples were examined by this validated method.

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Acknowledgments

This work was supported by the National Natural Science Foundation of China (No.20621502), the Scientific Technology Project of Guangdong Province (No.2005B33701012), and Medical Science Foundation of Guangdong Province (No.A2007072).

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Authors and Affiliations

  1. Centre for Disease Prevention and Control of Guangdong, Guangzhou, 510300, China

    Ximei Wu

  2. College of Chemistry and Molecular Sciences, Wuhan University, Luojiashan, Wuhan, 430072, China

    Ximei Wu

  3. Centre for Disease Prevention and Control of Guangdong, 176 Xingang West Road, Guangzhou, 510300, China

    Weixiong Huang, Lin Lu & Xingfen Yang

  4. State Key Laboratory of Biocontrol/MOE Key Laboratory of Aquatic Product Safety School of Life Sciences, Sun Yat-Sen University, Guangzhou, Guangdong, 510275, China

    Li Lin

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  1. Ximei Wu
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  2. Weixiong Huang
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  4. Li Lin
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Correspondence to Ximei Wu.

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Wu, X., Huang, W., Lu, L. et al. Simultaneous determination of six alkaloids in blood and urine using a hydrophilic interaction liquid chromatography method coupled with electrospray ionization tandem mass spectrometry. Anal Bioanal Chem 398, 1319–1327 (2010). https://doi.org/10.1007/s00216-010-4031-y

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  • DOI: https://doi.org/10.1007/s00216-010-4031-y

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