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Monitoring of Forbidden Medicines as Adulterants in Dietary Supplements Marketed Online by HPLC and ESI-tandom Mass Spectrometry

HPLC 및 ESI-tandom Mass Spectrometry를 이용한 인터넷에서 판매되는 기능성표방식품 중 부정유해물질 모니터링

  • Lee, Yong-Cheol (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Bog-Soon (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Yun, Eun-Sun (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Sung-Dan (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Chang, Min-Su (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Park, Young-Ae (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Shin, Young (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Jung, Sun-Ok (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Lee, Jae-In (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Chae, Young-Zoo (Seoul Metropolitan Government Research Institute of Public Health and Environment)
  • 이용철 (서울특별시 보건환경연구원) ;
  • 김복순 (서울특별시 보건환경연구원) ;
  • 윤은선 (서울특별시 보건환경연구원) ;
  • 김성단 (서울특별시 보건환경연구원) ;
  • 장민수 (서울특별시 보건환경연구원) ;
  • 박영애 (서울특별시 보건환경연구원) ;
  • 신영 (서울특별시 보건환경연구원) ;
  • 정선옥 (서울특별시 보건환경연구원) ;
  • 이재인 (서울특별시 보건환경연구원) ;
  • 채영주 (서울특별시 보건환경연구원)
  • Received : 2011.08.29
  • Accepted : 2012.01.18
  • Published : 2012.04.30

Abstract

It was carried out to detect anti-impotence drug-like compounds, sibutramine and their analogues in dietary supplements, which are doubtful whether they include illegal compounds. A total of 51 food products were bought online and have been investigated. The separation was achieved on a C18 column, with the mobile phase made up of water (5 mM sodium hexanesulfonate and 0.1% phosphoric acid) and 95% acetonitrile, at a flow rate of 1.2 mL/min with gradient elution using by HPLC-DAD. The UV signals were monitored at 220 nm and 291 nm. LC-ESI-tandom MS was utilized to confirm that detected compounds in samples are the same as the reference materials. Two nutrient supplement foods and ginseng products were found to contain 1.3-82.1 mg of sildenafil, dimethylthiolsildenafil and pseudovardenafil per serving size. In addition, two other processed products were detected to contain 1.7 and 2.2 mg of didesmethylsibutramine, derived from sibutramine per serving size.

인터넷에서 판매되는 건강기능성표방식품 51개를 구매하여 발기부전치료제 5종과 그 유사물질 29종, 이카린, 요힘빈, 시부트라민 그리고 시부트라민 유사물질인 데스메틸시부트라민, 디데스메틸시부트라민 총 39종의 부정유해물질을 3개의 혼합표준용액으로 만든 후 HPLC를 이용하여 총 50분 동안 이동상 용액 A(5 mM sodium hexanesulfonate와 0.1% phosphoric acid을 함유한 물), B(95% acetonitrile) 두 가지를 기울기 용매 조건으로 분석하였다. 검출된 화합물의 확인을 위하여 LC-ESI-tandom MS의 MRM 조건을 최적화하고 정성분석 한 결과 1개의 홍삼제품과 영양보충용제품 2건에서 실데나필과 슈도바데나필, 디메틸티오실데나필성분이 1회 복용량당 1.3-82.1 mg 검출되었으며, 2개의 기타가공품에서 부작용이 우려되어 사용이 금지된 시부트라민의 유사물질인 디데스메틸시부트라민이 각각 1회 복용량 당 2.2, 1.7 mg이 검출되었다. 시중에 판매되는 비아그라의 실데나필 1회 최소복용량은 25 mg으로 시료에서의 검출량은 이보다 높은 수준으로 함유되었으며, 의사의 처방 없이 식품 중에 불법적으로 함유된 이들 물질 혹은 이들의 유사물질은 소비자들의 건강상에 문제를 일으킬 수 있으므로, 시중에 유통되는, 더욱이 온라인 상에서 음성적으로 판매되고 있는 건강관련식품에 대한 모니터링이 지속적으로 필요한 실정이다.

Keywords

References

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