Chinese Journal of Chromatography ›› 2014, Vol. 32 ›› Issue (6): 586-590.DOI: 10.3724/SP.J.1123.2014.03001

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Determination of α-solanine,α-chaconine and solanidine in plasma and urine by ultra-performance liquid chromatography-triple quadrupole mass spectrometry

ZHANG Xiuyao, CAI Xinxin, ZHANG Xiaoyi   

  1. Wenzhou Center for Disease Control and Prevention, Wenzhou 325001, China
  • Received:2014-03-03 Revised:2014-03-26 Online:2014-06-08 Published:2014-05-22

Abstract:

An ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) method was developed for the determination of α-solanine,α-chaconine and solanidine in plasma and urine. The sample was acidified with aqueous solution containing 2% (v/v if not specified) formic acid, and then cleaned-up by solid-phase extraction with a mixed-mode cation exchange (MCX) cartridge. The analysis of the glycoalkaloids was carried out on an Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution of acetonitrile (containing 0.1% formic acid) and H2O (containing 0.05% formic acid and 5.0 mmol/L ammonium acetate). The analytes were detected by positive electrospray ionization tandem mass spectrometry in MRM mode, and quantified by external matrix-matched standard calibration. The cycle time of each analysis was 5.5 min. The calibration curves were linear in the range of 0.3-100 ng/mL of the glycoalkaloids in plasma and urine. The correlation coefficients were 0.997-0.999. The limits of detection (S/N=3) and quantitation (S/N=10) were 0.1 ng/mL and 0.3 ng/mL. The average recoveries were 82%-112% and 96%-114% for the glycoalkaloids spiked in plasma and urine, respectively, with relative standard deviations of 4.0%-16% and 2.7%-17% (n=6). The method is simple, accurate and sensitive to detect the glycoalkaloids in plasma and urine for both clinical and forensic purposes.

Key words: α-chaconine, α-solanine, plasma, potato, solanidine, tandem mass spectrometry, ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS), urine

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