TY - JOUR
T1 - Confirmatory analysis of malachite green, leucomalachite green, crystal violet and leucocrystal violet in salmon by liquid chromatography-tandem mass spectrometry
AU - Dowling, Geraldine
AU - Mulder, Patrick P.J.
AU - Duffy, Conor
AU - Regan, Liam
AU - Smyth, Malcolm R.
PY - 2007/3/14
Y1 - 2007/3/14
N2 - A method has been developed to analyse for malachite green (MG), leucomalachite green (LMG), crystal violet (CV) and leucocrystal violet (LCV) residues in salmon. Salmon samples were extracted with acetonitrile:McIIIvain pH 3 buffer (90:10 v/v), sample extracts were purified on a Bakerbond strong cation exchange solid phase extraction cartridge. Aliquots of the extracts were analysed by LC-MS/MS. The method was validated in salmon, according to the criteria defined in Commission Decision 2002/657/EC. The decision limit (CCα) was 0.17, 0.15, 0.35 and 0.17 μg kg-1, respectively, for MG, LMG, CV and LCV and for the detection capability (CCβ) values of 0.30, 0.35, 0.80 and 0.32 μg kg-1, respectively, were obtained. Fortifying salmon samples (n = 6) in three separate assays, show the accuracy to be between 77 and 113% for MG, LMG, LCV and CV. The precision of the method, expressed as RSD values for the within-laboratory reproducibility, for MG, LMG and LCV at the three levels of fortification (1, 1.5 and 2.0 μg kg-1), was less than 13%. For CV a more variable precision was obtained, with RSD values ranging between 20 and 25%.
AB - A method has been developed to analyse for malachite green (MG), leucomalachite green (LMG), crystal violet (CV) and leucocrystal violet (LCV) residues in salmon. Salmon samples were extracted with acetonitrile:McIIIvain pH 3 buffer (90:10 v/v), sample extracts were purified on a Bakerbond strong cation exchange solid phase extraction cartridge. Aliquots of the extracts were analysed by LC-MS/MS. The method was validated in salmon, according to the criteria defined in Commission Decision 2002/657/EC. The decision limit (CCα) was 0.17, 0.15, 0.35 and 0.17 μg kg-1, respectively, for MG, LMG, CV and LCV and for the detection capability (CCβ) values of 0.30, 0.35, 0.80 and 0.32 μg kg-1, respectively, were obtained. Fortifying salmon samples (n = 6) in three separate assays, show the accuracy to be between 77 and 113% for MG, LMG, LCV and CV. The precision of the method, expressed as RSD values for the within-laboratory reproducibility, for MG, LMG and LCV at the three levels of fortification (1, 1.5 and 2.0 μg kg-1), was less than 13%. For CV a more variable precision was obtained, with RSD values ranging between 20 and 25%.
KW - Crystal violet
KW - Leucocrystal violet
KW - Leucomalachite green
KW - Malachite green
KW - Method validation
KW - Salmon
UR - http://www.scopus.com/inward/record.url?scp=33846977744&partnerID=8YFLogxK
U2 - 10.1016/j.aca.2006.08.045
DO - 10.1016/j.aca.2006.08.045
M3 - Article
C2 - 17386742
AN - SCOPUS:33846977744
SN - 0003-2670
VL - 586
SP - 411
EP - 419
JO - Analytica Chimica Acta
JF - Analytica Chimica Acta
IS - 1-2 SPEC. ISS.
ER -