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Validation and Determination of Vet Drug Residues in Food and Feeding
Stuff considering as Example of Coccidiostats by LC-MS-MS |
| Introduction |
GALAB Laboratories is an international operating service provider of quality control
analysis for food and feeding stuff products. Our highly qualified staff, modern accredited
laboratories and state-of-the-art in analytical instrumentation guarantee best quality of
our services. Our commitment to customer demands and satisfaction make us a reliable
and sustained partner for the food and industry as well as the authorities.
GALAB Laboratories provides a wide range of vet drug residue analysis in different
matrices at lowest levels for high product safety.
Antibiotics are mainly used in food and for the treatment of bacterial diseases.
As there is a wide spectrumof antibiotics the need to detect these compounds at
very sensitive levels comes more and more into focus for the food and feeding stuff
industry. Annex 3 of the Council Directive 2377/90 compounds are listed with
maximum residue limits (MRLs) in different matrices for e.g. sulfonamides, tetracyclines,
quinolones. In Annex 4 MRLs could not be elaborated which means a zero tolerance in all foodstuffs of animal origin for e.g. nitrofuran metabolites, chloramphenicol,
imidazoles. The presence of these compounds at trace level and the complexity of
different matrices requires very sensitive methods of determination. According to the
German Foodstuff Law of 2003 lasalocid must not be used in feeding stuff to laying hens
older than 16 weeks. The aimof the developed method was to establish a method for
the reliable detection of coccidiostats, e.g. lasalocid in food and animal feed.
The poster shows an example of a contamination of feeding stuff and eggs at trace level
by coccidiostats incl. method validation according to DIN ISO 32645 and Council
Directive 96/23/EC. LC-MS-MS technique offers the possibility to develop sensitive and
specific residue methods to ensure the quality of food and feeding stuff products.
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| Experiments |
| Feedingstuff: Extraction/clean-Up of coccidiostats |
• 2 g sample
• NaOH
• ethylacetate
• cyclohexane
• SEC
• LC-MS-MS
(API 4000)
|
Real feeding stuff sample containing lasalocid of a concentration of
3.5 µg/kg, four transitions of lasalocid
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| Food: Extraction/clean-Upof coccidiostats |
• 2 g sample
• H2O/ NaOH
• ethylacetate
• cyclohexane
• SEC
• LC-MS-MS
(API 4000) |
Real egg sample containing lasalocid of a concentration of 1.5 µg/kg,
four transitions of lasalocid
|
| Validation data |
Method validation data for the coccidiostats determination were calculated following DIN ISO 32645 and Council Directive 96/23 EC. The ccα and ccβ values were evaluated by equidistant matrix sample calibration experiments. The application range for all shown coccidiostats in food and animal feed is between 1.0 and 20 µg/kg. The recovery rates for the coccidiostats in this validation are in the range of 61 to 70%.
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| Validation Data of Coccidiostats in Food and Feeding Stuff |
| compound |
cc α |
cc β |
LOD |
IDL |
precision |
recovery |
| |
[µg/kg] |
[µg/kg] |
[µg/kg] |
[µg/kg] |
VC [%] |
[%] |
| feeding stuff |
|
| Lasalocid |
0.11 |
0.22 |
0.11 |
0.22 |
1.1 |
68 |
| Narasin |
0.22 |
0.44 |
0.22 |
0.44 |
1.9 |
61 |
| Salinomycin |
0.18 |
0.35 |
0.18 |
0.35 |
2.1 |
70 |
| Monensin |
0.19 |
0.38 |
0.19 |
0.38 |
2.0 |
69 |
| egg |
|
| Lasalocid |
0.18 |
0.37 |
0.18 |
0.37 |
1.7 |
61 |
| Narasin |
0.18 |
0.36 |
0.18 |
0.36 |
1.6 |
67 |
| Salinomycin |
0.16 |
0.32 |
0.16 |
0.32 |
1.5 |
62 |
| Monensin |
0.08 |
0.16 |
0.08 |
0.16 |
0.7 |
70 |
|
|
LOD = limit of detection, IDL = identification limit: according to DIN ISO 32645
VC [%] = variation coefficient
ccα, ccβ according to Council Directive 96/23/EC
|
| Conclusion |
A highly sensitive and specific LC-MS-MS method for the quantitative determination of
four coccidiostats (lasalocid, monensin, salinomycin and narasin) in food and feeding
stuff has been developed and validated according to the Council Directive 96/23/EC and
DIN ISO 32645. The Identification limit ( IDL) for the coccidiostats are in the range of
0.16 to 0.44 µg/kg. Lowest concentrations of coccidiostats are detectable by using LC-MS-MS.
GALAB Laboratories offers a highly sensitive method for the determination of
coccidiostats in food and feeding stuff for a high product safety.
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