Determination of ionophore coccidiostats in feeding stuffs by liquid chromatography-tandem mass spectrometry. Part II. Application to cross-contamination levels and non-targeted feed.
A fit to purpose multi-analyte method for the official control of six coccidiostats (monensin sodium, salinomycin sodium, narasin, lasalocid sodium, semduramicin sodium and maduramicin ammonium alpha) at cross-contamination concentration levels in poultry, cattle, pig and calf compound feed by liquid chromatography tandem mass spectrometry (LC-MS/MS) has been developed and in-house validated. The corresponding maximum levels have been recently introduced by European legislation. The method developed involved a simple extraction of the coccidiostats from the feed samples followed by centrifugation and filtration of the supernatants for all matrices. For calf feed an additional de-fattening step of the filtrated supernatants with n-hexane was necessary. The resulting supernatants were submitted to chromatographic analysis. The analytes were quantified by a modified approach of the standard additions technique applied to the extracts, hence allowing a workload comparable to matrix-matched standard calibration curves. A further simplification of this technique was reached by applying the same addition levels of the target analytes for different concentration ranging from 0.5× maximum level up to 2.5× maximum level (universal approach). The concentration independent intermediate precision expressed in terms of relative standard deviation varied between 3 and 12% (except for maduramicin ammonium alpha and semduramicin sodium up to 21%) and the recovery rates ranged from 80 to 111%, depending on the target analyte and matrix. The limits of detection (LOD) and limits of quantification (LOQ) were different for the various analyte/matrix/instrument combinations but all LOQs were in the 0.01-0.65 mg kg(-1) range, hence well below the target concentrations of each analyte. Based on the obtained method performance characteristics the method is considered fit for the intended purpose.
European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Retieseweg 111, B-2440 Geel, Belgium. ursula.vincent@ec.europa.eu
Ursula
U
Vincent
Zigmas
Z
Ezerskis
Mostafa
M
Chedin
Christoph
C
von Holst
D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D002138:Calibration; D002417:Cattle; D002853:Chromatography, Liquid; D003049:Coccidiostats / Q000032:analysis* / Q000737:chemistry; D005506:Food Contamination; D007476:Ionophores / Q000032:analysis*; D057230:Limit of Detection; D011200:Poultry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization; D013552:Swine; D053719:Tandem Mass Spectrometry
D003049:Coccidiostats; D007476:Ionophores