title: Determination of atractyloside in Callilepis laureola using solid-phase extraction and liquid chromatography-atmospheric pressure ionisation mass spectrometry.
abstract: A selective analytical method based on high-performance liquid chromatography, combined with atmospheric pressure ionisation mass spectrometry, was developed for the detection of atractyloside. The analysis was performed on an Xterra Phenyl column utilising a gradient elution profile and a mobile phase consisting of 10 mM aqueous ammonium acetate buffer-methanol-acetonitrile. The calibration curve of the method (1 ng/ml-160 microg/ml) was best described by a second order polynomial function (r2 = 0.998) but displayed good linearity in the range of 100 ng/ml-1 microg/ml (r2 = 0.999). The limit of detection for the atractyloside standard was determined and found to be 100 pg/ml and the limit of quantification of atractyloside in tuber matrix was found to be 250 pg/ml. The relative standard deviation of the method was on average below 5% (n = 8). The method was successfully applied to the analysis of Callilepis laureola tubers and unknown powdered samples for the presence of atractyloside.
authors.affiliation: Forensic Chemistry Laboratory, Department of Health, Johannesburg 2000, South Africa. fcljhb@icon.co.za
authors.forename: Paul A
authors.initials: PA
authors.lastname: Steenkamp
authors.forename: Nial M
authors.initials: NM
authors.lastname: Harding
authors.forename: Fanie R
authors.initials: FR
authors.lastname: van Heerden
authors.forename: Ben-Erik
authors.initials: BE
authors.lastname: van Wyk
mesh_terms: D001274:Atmospheric Pressure; D036084:Callilepis / Q000737:chemistry*; D017022:Flow Injection Analysis; D013058:Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity