Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Establishment of Analytical Methods for Melamine Related Compounds in Biological Samples

생체시료 중 멜라민 화합물의 미량분석법 개발연구

  • Han, Kyoung-Moon (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Kim, Jin-Ho (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Cho, Soo-Yeul (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Shim, Sun-Bo (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Lee, Jin-Hee (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Lee, Ji-Hyun (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Hwang, In-Sun (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Kim, Sung-Il (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Cho, Yang-Ha (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Chai, Gap-Yong (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Kwon, Soon-Jae (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex) ;
  • Lee, Jun-Ho (National Institute of Food And Drug Safety Evaluation, Toxicological Evaluation and Research Department, Advanced Analysis Team Osong Health Technology Administration Complex)
  • 한경문 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 김진호 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 조수열 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 심선보 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 이진희 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 이지현 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 황의선 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 김성일 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 조양하 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 채갑용 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 권순재 (식품의약품안전평가원 독성평가연구부 첨단분석팀) ;
  • 이준호 (식품의약품안전평가원 독성평가연구부 첨단분석팀)
  • Received : 2010.08.30
  • Accepted : 2011.05.03
  • Published : 2011.06.30
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Abstract

Melamine has raised international concerns for its catastrophic health effects from tainted infant formula. This report concerns the developmental validation of a sensitive HPLC/MS/MS and GC/MS methods about melamine and cyanuric acid in human urine and serum. Analytical detection ranges of LC/MS was from 0.2 to 5.0 ng/mL and 2.0 to 60.0 ng/mL about melamine and cyanuric acid, respectively. The limits of quantification and confirmation are 0.2 ng/mL for both analytes in human urine and serum by LC/MS/MS. The range of recovery was 91.6%, and 107.6% for cyanuric acid and melamine in urine, respectively. The range of precision coefficient variation was from 2.0%, to 11.8% for cyanuric acid and melamine in urine. The range of recovery was from 94.9%, to 119.0% about cyanuric acid and melamine in serum, respectively. The range of precision coefficient variation from was 3.7%, and 13.5% about cyanuric acid and melamine in serum. Analytical detection ranges of GC/MS were 5.0 to 100.0 ng/mL about melamine and cyanuric acid, respectively. The limits of quantification and confirmation are 5.0 ng/mL for both analytes in human urine and serum by GC/MS. The range of recovery was from 83.7%, to 114.5% for cyanuric acid and melamine in urine, respectively. The range of precision coefficient variation was 3.5%, and 10.7% for cyanuric acid and melamine in urine. The range of recovery was 94.4%, and 110.7% for cyanuric acid and melamine in serum, respectively. The range of precision coefficient variation from was 3.9%, and 13.8% for cyanuric acid and melamine in serum. Several changes were taken to optimize performance by this method.

본 연구에서는 비료나 수지의 원료물질로 알려진 멜라민이 최근 수입식품 및 가공식품 등에서 검출되어 국제적으로 문제가 되어 생체시료 중 멜라민의 분석법을 확립하고 벨리데이션을 실시하여 신뢰성을 확보하고자 하였다. 생체시료(뇨 및 혈액) 중 멜라민 및 시아누르산 분석을 위해 단백질 침전법, 액체상 추출법으로 불순물을 제거하였고 LC/MS를 이용한 멜라민 최적분석법의 벨리데이션 결과에서 검출한계는 0.2 ng/mL(멜라민), 2.0 ng/mL(시아누르산)이었으며 각 정량범위내의 직선성은 0.9990이상을 가졌다. 뇨및 혈 중 멜라민의 quality control 시료는 0.5 ng/mL, 0.8 ng/mL, 2.0 ng/mL, 3.0 ng/mL으로서 뇨 중 멜라민 및 시아누르산의 정확성은 91.6%-107.6%범위를 나타내었고 정밀성은 2.0%-11.8%으로 나타났다. 혈 중 멜라민 및 시아누르산의 정확성은 94.9%-119.0%범위를 나타내었고 정밀성은 3.7%-13.5%으로 나타났다. 또한, GC/MS를 이용한 멜라민 분석의 검출한계는 5.0 ng/mL(멜라민), 5.0 ng/mL(시아누르산)이었고, 뇨 및 혈중 멜라민의 quality control 시료는 10.0~40.0 ng/mL이었으며, 뇨 및 혈 중 멜라민 및 시아누르산의 정확성은 83.7%~ 10.7% 범위를 나타내었고, 정밀성은 3.5%-13.8% 으로 나타났다.

Keywords

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