4.5 Article

Optimisation and validation of ultra-high performance liquid chromatographic-tandem mass spectrometry method for qualitative and quantitative analysis of potato steroidal alkaloids

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ELSEVIER
DOI: 10.1016/j.jchromb.2015.05.033

关键词

Potato; Steroidal alkaloids; Validation; Multiple reaction monitoring; UHPLC-MS/MS

资金

  1. NovTechIng project - Food Institutional Research Measure of the Irish Department of Agriculture, Food and Marine [FIRM 11/F/050]

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An ultra-high performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS) method for quantification of potato steroidal alkaloids, namely alpha-solanine, alpha-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 C-18 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 0.001-0.004 mu g/mL whereas the linearities of the standard curves were between 0.980 and 0.995. (C) 2015 Elsevier B.V. All rights reserved.

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