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여름정기학술대회

2022여름초록

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Development and validation of modified QuEChERS method coupled with UPLC–MS/MS for simultaneous determination of chloramphenicol, thiamphenicol, florfenicol, and its metabolite

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건국대학교
발표구분
포스터발표
포스터발표
3. Food & Environment
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Amphenicols are widely used in livestock and poultry breeding and production. This study aimed to develop a validated method for simultaneous quantification of chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF), and florfenicol amine (FFA) residues in beef, pork, chicken, flatfish, eel, and shrimp using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with UPLC-MS/MS. Primary-secondary amine (PSA) and MgSO4 were used for sample purification. The analytes were separated on a reversed-phase analytical column and mobile phase consisting of (A) distilled water and (B) acetonitrile with 0.1% acetic acid were used to achieve optimal chromatographic separation. Matrix matched standard calibration curves (R2≥0.9941) were obtained for concentration equivalent to ×1/2, ×1, ×2, ×3, ×4, and ×5 fold the maximum residue limit (MRL) stipulated by the Korean Ministry of Food and Drug Safety (KMFDS). The KMFDS has banned the use of CAP in animal products. Thus, it was analyzed based on the minimum required performance limit (MRPL) of KMFDS. Recoveries of 64.3~116.5%, with relative standard deviations (RSDs) of ≤18.05% (intraday and interday), were obtained for each sample at three spiking concentrations (CAP:×1/2, and ×6 the MRPL values; TAP, FF,, and FFA:×1/2, ×1 and ×2 the MRL values). The calculated limits of detection (LODs) and limits of quantification (LOQs) were 0.005–3.1 and 0.02–10.4 μg/kg, respectively. The developed method was successfully applied for monitoring samples obtained from local markets in Seoul, Republic of Korea. 

The study was supported by the Ministry of Food and Drug Safety Administration, Republic of Korea [grant number 20162MFDS621] in 2020.


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