title: Optimisation and validation of ultra-high performance liquid chromatographic-tandem mass spectrometry method for qualitative and quantitative analysis of potato steroidal alkaloids.
abstract: An ultra-high performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS) method for quantification of potato steroidal alkaloids, namely α-solanine, α-chaconine, solanidine and demissidine was developed and validated. Three different column chemistries, i.e. ethylene bridged hybrid (BEH) C18, hydrophilic lipophilic interaction and amide columns, were assessed. The BEH C18 column showed best separation and sensitivity for the alkaloids. Validation data (inter-day and intra-day combined) for accuracy and recovery ranged from 94.3 to 107.7% and 97.0 to 103.5%, respectively. The accuracy data were within the acceptable range of 15% as outlined in the United States Food and Drug Administration (USFDA) guidelines. The recovery data were consistent and reproducible with a coefficient of variation (CV) ranging from 6.2 to 9.7%. In addition, precision of the method also met the criteria of the USFDA with CV values lower than 15% even at lower limit of quantification (LLOQ), while the permissible variation is considered acceptable below 20%. The limit of detection and LLOQ of the four alkaloids were in the range of 0.001-0.004μg/mL whereas the linearities of the standard curves were between 0.980 and 0.995.
authors.affiliation: Food Biosciences Department, Teagasc Food Research Centre Ashtown, Dublin 15, Ireland.
authors.forename: Mohammad B
authors.initials: MB
authors.lastname: Hossain
authors.affiliation: Food Biosciences Department, Teagasc Food Research Centre Ashtown, Dublin 15, Ireland. Electronic address: dilip.rai@teagasc.ie.
authors.forename: Dilip K
authors.initials: DK
authors.lastname: Rai
authors.affiliation: School of Agriculture and Food Science, University College Dublin, Dublin 4, Ireland.
authors.forename: Nigel P
authors.initials: NP
authors.lastname: Brunton
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D016014:Linear Models; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012991:Solanaceous Alkaloids / Q000032:analysis* / Q000737:chemistry; D011198:Solanum tuberosum / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D012991:Solanaceous Alkaloids
keywords: Multiple reaction monitoring; Potato; Steroidal alkaloids; UHPLC–MS/MS; Validation