Anthelmintic drug residues in beef: UPLC-MS/MS method validation, European retail beef survey, and associated exposure and risk assessments

Abstract

Anthelmintic drugs are widely used to control parasitic infections in cattle. The ProSafeBeef project addressed the need for data on the exposure of European consumers of beef to potentially harmful drug residues. A novel analytical method based on matrix solid-phase dispersive extraction and ultra-performance liquid chromatography-tandem mass spectrometry was validated for 37 anthelmintic drugs and metabolites in muscle (assay decision limits, CCα, = 0.15-10.2 µg kg⁻¹). Seven European countries (France, Spain, Slovenia, Ireland, Italy, Belgium and Portugal) participated in a survey of retail beef purchased in local shops. Of 1061 beef samples analysed, 26 (2.45%) contained detectable residues of anthelmintic drugs (0.2-171 µg kg⁻¹), none above its European Union maximum residue limit (MRL) or action level. Residues detected included closantel, levamisole, doramectin, eprinomectin, moxidectin, ivermectin, albendazole and rafoxanide. In a risk assessment applied to mean residue concentrations across all samples, observed residues accounted for less than 0.1% of the MRL for each compound. An exposure assessment based on the consumption of meat at the 99th percentile of consumption of adults in 14 European countries demonstrated that beef accounted for less than 0.02% of the acceptable daily intake for each compound in each country. This study is the first of its kind to apply such a risk-based approach to an extensive multi-residue survey of veterinary drug residues in food. It has demonstrated that the risk of exposure of the European consumer to anthelmintic drug residues in beef is negligible, indicating that regulation and monitoring is having the desired effect of limiting residues to non-hazardous concentrations.

Evolution and applications of the QuEChERS method

“…As a consequence, pharmaceutical-compound analysis is also an active analytical area, in which fast, feasible analytical methods are required, especially in food control and safety. In this sense, the application of the QuEChERS method was demonstrated to be successful (see Table 2 for some examples), for the separate determination of certain families of drugs {e.g., sulfonamides [54], quinolones [55], anthelmintics [19,56,[57][58][59], or benzimidazoles [60]} and to carry out multi-residue analysis [61][62][63][64][65].…”

“…As usual, the separation technique most widely applied for pharmaceutical compounds analysis in combination with QuEChERS is LC, both HPLC [54,61,66] and UHPLC [56][57][58][59][60]63,64]. Even capillary LC [55] or GC (less common) [65] have been selected.…”

“…Even capillary LC [55] or GC (less common) [65] have been selected. In most cases and as desirable, these techniques have been coupled to MS detection systems [19,54,[56][57][58][59][60][61][63][64][65][66]. In certain cases, the determination of the target analytes was carried out without previous chromatographic separation by DART [62] -for example, the work of Martínez-Villalba et al [62], who carried out the determination of a group of 20 benzimidazoles in milk and four coccidiostats in feed.…”

Potential impacts of climate change on veterinary medicinal residues in livestock produce: An island of Ireland perspective††This paper is one of a series of reviews on “Climate Change and Food Safety – an Island of Ireland perspective”.

“…According to Bennema et al (2010) 59% of dairy herds in Ireland use preventative anthelmintics compared with 17% in United Kingdom (UK) and 6% in Germany. This high usage is reflected in a study showing that of seven European countries Ireland had the highest incidence of anthelmintic drug residues in locally purchased beef, albeit within permitted limits (Cooper et al, 2012). Application of anthelmintics, usually once or twice per year, is ingrained in the farming culture of IoI and they are one of the most commonly administered veterinary livestock drugs in this region.…”

“…This gap has largely been filled by closantel, either as a single active or in combination with ivermectin, its use increasing from 22% by 2005 to 56% by 2011 (McMahon et al, 2013b). Closantel's popularity is demonstrated by it being the most common anthelmintic residue detected in a survey of beef purchased in ROI in 2009(Cooper et al, 2012.…”