본 연구는 국내 생산 및 수입 양식 수산물에 대해 잔류 할 수 있는 향정신성 의약품인 디아제팜 대한 안전관리 강화기반을 위해 마련되었다. 중국인민공화국 국가 표준 시험법(GB 29697-2013)을 기반으로 전처리 방법을 개선 하여 GC-MS/MS 시험법을 확립하였으며, LC-MS/MS 방 법과의 기기간 검증을 통해 확립된 시험법의 선택성, 정량한계 및 회수율에 대한 검증을 통해 디아제팜 시험법으로서의 유효성을 확인하였다. LC-MS/MS의 경우 아세토니트릴로 추출 후 PSA를 이용해 정제하였고, GC-MS/MS의 경우 아세토니트릴로 추 출후 C18카트리지를 이용해 정제하였다. 디아제팜은 표준용액을 정량한계를 포함한 농도에 따라 검량선을 작성한 결과 두 기기 모두 r2> 0.99 이상의 직선성을 확인하였다. 본 실험에서의 검출한계와 정량한계는 LC-MS/MS 및 GCMS/ MS 모두 0.0004 mg/kg, 0.001 mg/kg 수준이었으며, 평균 회수율은 각각 99.8~106%, 109~124%이었다. 또한, 분석오차는 모두 15% 이하로 정확성 및 재현성이 우수하였 으며, CODEX 가이드라인 규정에 만족하는 수준이었다. 따라서 개발된 시험법은 안전한 수산물의 국내 유통과 잔 류실태조사를 위해 활용될 것으로 기대한다.

The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/ MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, r 2 was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

ABSTRACT
 Materials and Methods
  시약 및 재료
  표준원액 및 표준용액의 조제
  추출 및 정제
  기기분석조건
  분석법 검증
 Results and Discussion
  LC-MS/MS를 이용한 분석법 선정 및 조건확립
  LC-MS/MS를 이용한 추출 및 정제조건 확립
  GC-MS/MS를 이용한 분석법 선정 및 조건확립
  GC-MS/MS를 이용한 추출 및 정제조건 확립
  분석법 검증
 Acknowledgement
 국문요약
 References

• 신다솜(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과, Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) | Dasom Shin
• 강희승(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과, Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) | Hui-Seung Kang Correspondence to
• 김주혜(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과, Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) | Joohye Kim
• 정지윤(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과, Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) | Jiyoon Jeong
• 이규식(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과, Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) | Gyu-Seek Rhee