본 연구에서는 2018년 충남지역에서 생산, 출하되는 수산물에 대해 잔류동물용의약품 실태를 조사하였다. 수산물 115건을 대상으로 식품공전 수산물 중 동물용의약품 동시 다성분 시험법으로 분석이 가능한 29종의 잔류동물 용의약품을 분석하였다. 115건의 수산물 중 9건에서 6종의 잔류동물용의약품이 검출되었으며, 검출률은 7.8%이었다. 검출된 잔류동물용의약품은 옥소린산, 엔로플록사신이 가장 많이 검출되었으며 시프로플록사신, 설파디아진, 플루메퀸, 옥시테트라사이클린이 각각 검출되었다. 미꾸라지 검체 1건에서 엔로플록사신이 잔류기준을 초과하였으나 전체적으로 안전한 수준으로 평가되었다. 그렇지만 잔류 동물용의약품 검출률이 높아지는 추세이고 종류 또한 다양해지고 있어 지속적인 모니터링이 필요하다.

HPLC-MS/MS를 이용하여 벌꿀의 동물용의약품 동시분석을 위한 분석법을 정립하고자 식품공전 중 벌꿀에 규격이 설정된 11종의 동물용의약품을 2개 그룹 Group 1 (streptomycine, dihydrostreptomycine, neomycine)과 Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate)으로 나눠서 동시에 분석 할 수 있는 방법을 연구 하였다. 두 그룹모두 RT는 15분 이내였고, 검출한계는 0.0056~0.0643 μg/g, 정량한계는 0.0169~0.1948 μg/g으로 나타났으며 Group 1 (0.05~1.0 μg/g의 농도범위)과 Group 2 (0.01~1.0 μg/mL) 의 검량선을 작성한 결과 각 동물용의약품의 직선상관계수(R2)는 0.9917~0.9987, 0.9923~1.000으로 매우 양호한 상태를 보였고, 최종 농도가 0.25 μg/g, 1.0 μg/g에서의 회수율은 Group 1 65.1~80.6%, Group 2 64.2~90.3%를 나타났다, 또한 area 및 RT 에 대한 inter (n = 3), intra day (n = 6) RSD (%) 분석결과는 area는 10.92%이하, RT은 1.57% 이하로 나타나 양호한 수준을 보여 벌꿀 중 동물용의약품동시분석 방법으로 적합하다고 판단된다.

A liquid chromatographic-tandem mass spectrometric (LC-MS/MS) multi-residue method for simultaneous quantification and identification of 37 anthelmintic veterinary drug residues (including benzimidazoles, macrocyclic lactones, and flukicides, levamisole, pyrantel and niclosamide) in milk has been developed and validated. For sample preparation, we used a simple modification of the QuEChERS (quick, easy, cheap, effective, rugged and safe) method, which was initially developed for analysis of pesticide residues. Anthelmintic residues were extracted into acetonitrile:methanol (9:1, v/v) using sodium chloride to induce liquid-liquid partitioning followed by dispersive solid phase extraction for cleanup. The extract was concentrated into dimethyl sulphoxide, which was used as a keeper to ensure that analytes remain in solution. Using rapid polarity switching in electrospray ionization, a single injection was capable of detecting both positively and negatively charged ions within a 15 min run time. The Limit of detection (LOD) and the Limit of quantification (LOQ) method ranged from 0.1 ng/g to 4.4 ng/g and from 0.3 ng/g to 14.6 ng/g, respectively. Validation of the developed method was based on international guidelines. Average recoveries ranged from 70% to 120%, except for 54.7% at 0.5× MRL (rafoxanide) and 69.0% at 0.5× MRL (closantel). The coefficient of variation for the described method was less than 15% over the range of concentrations studied. The result of the method was verified successfully by participation in a proficiency study for analysis of anthelmintic drugs.

The Korean National Residue Program consists of three sampling plans for domestic and imported foods of animal origin : monitoring, surveillance/enforcement and exploratory testing. Monitoring and surveillance/enforcement testing programs are routinely implemented by 17 Provincial Veterinary Services for domestic products and two regional offices of Animal, Plant and Fisheries Quarantine and Inspection Agency (QIA) for imported products, respectively. The exploratory testing is designed to test substances which are not included in the list of monitoring and enforcement testing programs controlled by headquarter of QIA. In 2010, the exploratory testing was carried out in domestic and imported foods of animal origin for 24 veterinary drugs including florfenicol, clavulanic acid, four quinolones (nalidixic acid, difloxacin, marbofloxacin, orbifloxacin), two anthelmintics (closantel, levamisole), two sedatives (azaperone, carazolol), six glucocorticoids (dexamethasone, betamethasone, flumethasone, prednisone, prednisolone, methylprednisolone), eight non-steroidal anti-inflammatory drugs (phenylbutazone, paracetamol, carprofen, flunixin, ketoprofen, meloxicam, tolfenamic acid, acetylsalicylic acid). In the total of 1,153 domestic samples, only florfenicol was detected from 17 pig muscles at levels of 0.2～614 ng/g. Of 17 positive pig muscles, 16 samples were non-violative and one sample was violative. In the total of 1,065 imported samples, florfenicol was detected at 0.4 ng/g in one pork. Also, flunixin was detected at 22 ng/g in one beef.