• 한국식품위생안전성학회지
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• 제31권2호
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• pp.85-93
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• 2016

미꾸라지에서의 Nitrofuran계 대사물질인3-amino-2-oxazolidone(AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone(AMOZ), 1-ammino-hydantoin (AHD)와 semicarbazide(SEM)의 잔류량을 검사하기 위해HPLC-MS/MS를 이용한 신속한 정량법이 개발되었다. 2-nitrobenzaldehyde (2-NBA)를 이용해 $50^{\circ}C$에서 1시간 동안 산 가수분해와 유도체화 과정을 거친 뒤에, 액-액 분배로 정제와 추출을 하였다. 회수율은 음성시료에 3가지 농도 0.5, 1.0, $2.0{\mu}g/kg$의 표준액을 첨가하여 평가하였고 평균 회수율은 75.1-108.1% 이었다. 정밀성(%RSD)은 일내 8.7% 이하, 일간 8.5% 이하였다. 직선성은 NBAOZ는 $0.2-20{\mu}g/Kg$, NBAMOZ는 $0.8-20{\mu}g/Kg$, NBAHD는 $0.2-20{\mu}g/Kg$, NBSEM 는 $0.1-20{\mu}g/Kg$ 범위에서 모두 상관계수 0.99이상이었다. 검출한계(LOD)는 NBAOZ $0.06{\mu}g/Kg$, NBAMOZ $0.24{\mu}g/Kg$, NBAHD $0.06{\mu}g/Kg$, NBSEM $0.03{\mu}g/Kg$이었고, 정량한계(LOQ)는 NBAOZ $0.2{\mu}g/Kg$, NBAMOZ $0.8{\mu}g/Kg$, NBAHD $0.2{\mu}g/Kg$, NBSEM $0.1{\mu}g/Kg$ 이었다. 가수분해 및 유도체화 소요시간을 1시간으로 줄여 만든 신속 간편한 이 시험법이 미꾸라지 중 nitrofuran metabolites잔류량 분석에 적합함을 확인할 수 있었다.

• 대한수의학회지
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• 제46권4호
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• pp.295-304
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• 2006

Residual materials such as veterinary drugs, environmental contaminants, and pesticides are affecting food safety. High resolution techniques and quality controls are needed to analyze these materials from part per million to part per trillion quantities in food. In order to achieve quality results, standardized methods and techniques are required. Our laboratories were prepared to obtain a certificate of accreditation for ISO/IEC 17025 in the analytical criteria of animal drugs, dioxins, pesticides, and heavy metals. ISO together with IEC has built a strategic partnership with the World Trade Organization with the common goal of promoting a free and fair global trading system. ISO collaborates with the United Nations Organization and its specialized agencies and commissions, particularly those involved in the harmonization of regulations and public policies including the World Health Organization and CODEX Alimentarius for food safety measurement, management and traceability. Our goal was to have high quality analysts, proper analytical methods, good laboratory facilities, and safety systems within guidelines of ISO/IEC 17025. All staff members took requirement exams. We applied proficiency tests in the analysis of veterinary drugs (nitrofuran metabolites, sulfonamide and tetracyclines), dioxins, organophosphorus pesticides, and heavy metals (Cd, Pb, As) to the Food Analysis Performance Assessment Scheme (FAPAS) at Central Science Laboratory, Department for Environment Food and Rural Affairs (DEFRA), England. The results were very satisfactory. All documents were prepared, including system management, laboratory management, standard operational procedures for testing, reporting, and more. The criteria encompassed the requirements of ISO/IEC 17025:1999. Finally, the Korea Laboratory Accreditation Scheme (KOLAS) accredited our testing laboratories in accordance with the provisions of Article 23 of the National Standards Act. The accreditation will give us the benefit of becoming a regional reference laboratory in Asia.