Validation of a Rapid Quantitative Method for the Residues of Nitrofuran Metabolites in Loach by Accelerated Solvent Extraction and HPLC Triple Quadrupole Mass Spectrometry

서지정보

· 발행기관 : 한국식품위생안전성학회
· 수록지 정보 : 한국식품위생안전성학회지 / 31권 / 2호
· 저자명 : Eun Chae Ryu, Yun-jeong Han, Seong-soo Park, Chul-joo Lim, Sunok Choi, Se Chang Park

목차

Materials and Methods
Reagents, Chemicals and Samples
Stock and Working Standard Solution
Extraction procedure
Chromatographic Separation Parameters
Instrumentation and Apparatus
Method Validation
Selectivity and Specificity
Linearity
Sensitivity (LOD, LOQ, CCα and CCβ)
Precision, Accuracy and Recovery
Results
Extraction Optimization
Optimization of LC-MS/MS Conditions
Method Validation
Selectivity and Specificity
Linearity
Sensitivity (LOD, LOQ, CCα and CCβ)
Precision, Accuracy and Recovery
Discussion
Acknowledgemen
국문 요약
References

초록

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℃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 μg/kg의 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 μg/Kg, NBAMOZ는 0.8-20 μg/Kg, NBAHD는 0.2-20 μg/Kg, NBSEM 는 0.1-20 μg/Kg 범위에서 모두 상관계수 0.99이상이었다. 검출한계(LOD)는 NBAOZ 0.06 μg/Kg, NBAMOZ 0.24 μg/Kg, NBAHD 0.06 μg/Kg, NBSEM 0.03 μg/Kg이었고, 정량한계(LOQ)는 NBAOZ 0.2 μg/Kg, NBAMOZ 0.8 μg/Kg, NBAHD 0.2 μg/Kg, NBSEM 0.1 μg/Kg 이었다. 가수분해 및 유도체화 소요시간을 1시간으로 줄여 만든 신속 간편한 이 시험법이미꾸라지 중 nitrofuran metabolites잔류량 분석에 적합함을 확인할 수 있었다.

영어초록

A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at 50℃, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and 2.0 μg/kg), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ≤ 8.7% and ≤ 8.5% for intra-day and inter-day precision, respectively. Linearity was studied in the range of 0.2-20 μg/Kg for NBAOZ, 0.8-20 μg/Kg for NBAMOZ, 0.2-20 μg/Kg for NBAHD, and 0.1- 20 μg/Kg for NBSEM, and the obtained coefficient correlations (r) were ≥ 0.99 for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at 0.06 μg/Kg for NBAOZ, 0.24 μg/Kg for NBAMOZ, 0.06 μg/Kg for NBAHD, and 0.03 μg/Kg for NBSEM. Limits of quantification (LOQs) were established at 0.2 μg/Kg for NBAOZ, 0.8 μg/Kg for NBAMOZ, 0.2 μg/Kg for NBAHD, and 0.1 μg/Kg for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitrofuran residues in loach.

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