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Determination of malachite green and leucomalachite green in carp muscle by liquid chromatography with visible and fluorescence detection
A liquid chromatography-VIS/FLD method for the analysis of malachite green (MG) and its major metabolite, leucomalachite green (LMG) in carp muscle has been described. The method consists in an extraction with acetonitrile-buffer mixture followed by partioning with dichloromethane. Clean up and isol...
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Published in: | Journal of Chromatography A 2005-09, Vol.1089 (1), p.187-192 |
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Main Authors: | , , |
Format: | Article |
Language: | English |
Subjects: | |
Citations: | Items that this one cites Items that cite this one |
Online Access: | Get full text |
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Summary: | A liquid chromatography-VIS/FLD method for the analysis of malachite green (MG) and its major metabolite, leucomalachite green (LMG) in carp muscle has been described. The method consists in an extraction with acetonitrile-buffer mixture followed by partioning with dichloromethane. Clean up and isolation were performed on SCX solid phase extraction (SPE) column. Chromatographic separation was achieved by using phenyl-hexyl column with an isocratic mobile phase consisting of acetonitrile and acetate buffer (0.05
M, pH 4.5) (60:40, v/v). Liquid chromatography with absorbance detector (
λ
=
620
nm) was used for the determination of MG while LMG was detected by fluorescence detector (
λ
ex
=
265
nm and
λ
em
=
360
nm). The both detectors were connected on-line which allowed direct analysis of a sample extract for MG and LMG without the need for any post-column procedure. The whole method has been validated, according to the EU requirements (Commission Decision 2002/657/EC). Specificity, stability, decision limit (CC
α), detection capability (CC
β), accuracy and precision were determined. Average recoveries of MG and LMG from muscle fortified at three levels (0.5, 1 and 2
μg/kg) were 62% (range from 60.4 to 63.5%) and 90% (range from 89.0 to 91.5%), respectively. Relative standard deviations (RSD) of recoveries at all fortification levels were less than 10.9 and 8.6% for MG and LMG, respectively. The calculated CC
α for MG and LMG were 0.15 and 0.13
μg/kg, and CC
β were 0.37 and 0.32
μg/kg, complying with the minimum required performance limit (MRPL) of 2
μg/kg (sum of MG and LMG). |
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ISSN: | 0021-9673 |
DOI: | 10.1016/j.chroma.2005.07.004 |