Comprehensive analysis of ß-lactam antibiotics including penicillins, cephalosporins, and carbapenems in poultry muscle using liquid chromatography coupled to tandem mass spectrometry

Abstract

A comprehensive method for the quantitative residue analysis of trace levels of 22 ß-lactam antibiotics, including penicillins, cephalosporins, and carbapenems, in poultry muscle by liquid chromatography in combination with tandem mass spectrometric detection is reported. The samples analyzed for ß-lactam residues are hydrolyzed using piperidine in order to improve compound stability and to include the total residue content of the cephalosporin ceftifour. The reaction procedure was optimized using a full experimental design. Following detailed isotope labeling, tandem mass spectrometry studies and exact mass measurements using high-resolution mass spectrometry reaction schemes could be proposed for all ß-lactams studied. The main reaction occurring is the hydrolysis of the ß-lactam ring under formation of the piperidine substituted amide. For some ß-lactams, multiple isobaric hydrolysis reaction products are obtained, in accordance with expectations, but this did not hamper quantitative analysis. The final method was fully validated as a quantitative confirmatory residue analysis method according to Commission Decision 2002/657/EC and showed satisfactory quantitative performance for all compounds with trueness between 80 and 110% and within-laboratory reproducibility below 22% at target level, except for biapenem. For biapenem, the method proved to be suitable for qualitative analysis only.

Comprehensive analysis of toxics (pesticides, veterinary drugs and mycotoxins) in food by UHPLC-MS

“…This issue was highlighted by Berendsen et al [31], who simultaneously determined penicillins, cephalosporins and carbapenems in poultry muscle. Moreover, some veterinary drugs need to be determined and confirmed at very low concentrations (<1 μg/kg).…”

Fast HPLC-MS/MS Method for Determining Penicillin Antibiotics in Infant Formulas Using Molecularly Imprinted Solid-Phase Extraction

“…These molecules derive their activity from the 6-aminopenicillanic acid nucleus which is effective against mainly Gram-positive bacteria ( Figure 1 ). Amoxicillin, ampicillin, penicillin G, penicillin V, cloxacillin, dicloxacillin, oxacillin, and nafcillin are registered drugs for the treatment of food-producing animals [ 3 ]. In dairy cattle, in addition to digestive and respiratory diseases, the inflammation of the mammary gland is very problematic for the farmer.…”

“…For this reason, fast and straightforward methods of determination are generally preferred [ 9 ]. High performance liquid chromatography (HPLC) has been the most frequent technique for analyzing penicillins and other BLAs in different matrices, usually coupled with mass spectrometry (MS) [ 1 , 3 , 7 , 10 , 11 ]. Usually, this technique implies previous clean-up steps using common solid-phase extraction (SPE) procedures.…”

Determination of Antibiotic Residues: II. Extraction and Clean-up Methods for Liquid Samples_A Review

“…또한 배출된 의약품 일부는 생물학적 활성도가 그대로 유지되기도 한다 (MartinezCarballo et al, 2007). Kroker (1983)는 돼지가 베타-락탐계 Martinez-Carballo et al, 2007;McArdell et al, 2003;Tolls, 2001 and Samanidou, 2013;Lopes et al, 2012;Xu et al, 2012), 육류 (Berendsen et al, 2013;Bousova et al 2013;Tao et al 2012), 가축사료 (Amelin and Timofeev, 2016;Boscher et al, 2010;Pietruk et al 2015) 등의 고체 시료를 대상으로 전처 리방법을 개발·적용한 사례가 있으나 가축분뇨 중의 항생제 분석방법 (Gorissen et al 2015;Zhou et al, 2012) (Chitescu et al, 2015;Gros et al, 2013;Iglesias et al, 2012;Shelver et al, 2010). 고상추출법은 일반적으로 Fig 편적으로 적용 가능한 최적 전처리조건을 도출하기 위한 다 양한 연구가 진행되어 왔다 (Ben et al, 2008;De Alwis and Heller, 2010;Gros et al, 2013;Iglesias et al, 2012;Zhou et al, 2012 (Ben et al, 2008;Gros et al, 2013;Shelver et al, 2010;Zhou et al, 2012) …”