Identification of "unknown analytes" in injection sites: a semi-quantitative interpretation

被引:5
作者
De Wasch, K
Van Hoof, N
Poelmans, S
Okerman, L
Courtheyn, D
Ermens, A
Cornelis, M
De Brabander, HF
机构
[1] Ghent Univ, Dept Vet Food Inspect, Fac Vet Med, B-9820 Merelbeke, Belgium
[2] State Lab Ghent, B-9050 Gentbrugge, Belgium
[3] Inst Vet Inspect, B-1040 Brussels, Belgium
关键词
liquid chromatography with mass spectrometry (LC-MSn); veterinary; maximum residue limit (MRL); phenylbutazone; penicillin G benzathine; florfenicol;
D O I
10.1016/S0003-2670(02)01031-0
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The analytical approach to the detection of residues of legally used veterinary medicinal products (VMPs) is similar to the approach of forbidden substances. The only difference lies in the quantitative component of the method. Since there is an evolution towards a different strategy in the screening for VMPs in matrices of slaughtered animals, a new approach was developed for determining the residues. The aim of this research was to create an efficient screening approach for determining the identity and/or quantity of legally and illegally used VMPs present at high concentrations in injection sites. The determination of these 'unknown' VMPs is combined with a fast report to the customer. Examples are given of the identification of phenylbutazone, penicillin G benzathine and florfenicol. For quantitative purposes, using a mini-validation procedure, concentrations far above the maximum residue limit (MRL) of the identified VMP can be reported. A quantitative validation normally consists of determining the required validation parameters at three levels: 1/2 MRL, MRL, 2 MRL. For highly concentrated injection sites, an alternative approach is proposed. The alternative validation consists of a comparison of the analyte concentration in the sample with the spike at the MRL and 10 times the MRL concentration. (C) 2002 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:387 / 399
页数:13
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