Determination of Six Sweeteners in Children's Favorite Foods by HPLC-MS/MS

HPLC-MS/MS를 이용한 어린이 기호식품중의 감미료 분석

  • Kim, Il-Young (Food Analysis Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Du, Ok-Ju (Food Analysis Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Lee, Sung-Dck (Food Analysis Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Park, Young-He (Food Analysis Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Mi-Sun (Food Analysis Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Bea, Chung-Ho (Food Analysis Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Chae, Young-Zoo (Food Analysis Team, Seoul Metropolitan Government Research Institute of Public Health and Environment)
  • 김일영 (서울특별시보건환경연구원 식품분석팀) ;
  • 두옥주 (서울특별시보건환경연구원 식품분석팀) ;
  • 이성득 (서울특별시보건환경연구원 식품분석팀) ;
  • 박영혜 (서울특별시보건환경연구원 식품분석팀) ;
  • 김미선 (서울특별시보건환경연구원 식품분석팀) ;
  • 배청호 (서울특별시보건환경연구원 식품분석팀) ;
  • 채영주 (서울특별시보건환경연구원 식품분석팀)
  • Received : 2010.02.01
  • Accepted : 2010.04.21
  • Published : 2010.06.30

Abstract

A HPLC-MS/MS method was developed for simultaneous determination of six sweeteners (acesulfame-K, cyclamate, saccharin, sucralose, stevioside, aspartame) in children's favorite foods. The procedure involves an extraction of the six sweeteners with 50% methanol solution, sample clean-up using the Carrez clearing reagent and filtering with cartridge filter. The HPLC separation was performed on a Hypersil Gold (150 mm ${\times}$ 2.1 mm 5 um) column using the water/acetonitrile mobile phase (95:5). Mass spectrometric analysis was carried out using the TSQ Quantum Ultra operated in negative and positive ESI/SRM. With this method, good linear relationship, sensitivity and reproducibility were obtained. The spike recoveries of six sweeteners for 2 kinds of foods spiked into 0.4 mg/ kg ranged from 87.4 to 114.7%. The detection limits were above 0.02 mg/kg. The method has been applied to determination of six sweeteners in children's favorite foods.

아세설팜칼륨, 싸이클라메이트, 삭카린나트륨, 수크랄로스, 스테비오사이드, 아스파탐을 HPLC/MS/MS를 이용하여 동시 분석한 결과 각 감미료 별로 고유한 스펙트럼을 얻어 정량하여 머므름 시간은 2.26~9.96로 10분 이내로 분석이 가능하였다. 각각 감미료의 상관계수($R^2$)은 0.9986~0.9999로 양호한 직선상의 그래프를 얻을 수 있었고 각각의 감미료를 단계적으로 희석하여 분석한 결과 검출한계는 아세설팜칼륨, 싸이클라메이트 삭카린나트륨, 수크랄로스, 스테비오사이트, 및 아스파탐의 경우 0.02 mg/kg이었다. 시료에 대한 6종의 감미료에 대한 분석법의 회수율은 과자 87.4~106.9%, 캔디 99.8~114.7%로 전반적으로 좋은 회수율을 보여 어린이기호식품에서의 감미료 분석에 적용하였다.

Keywords

References

  1. 문범수 : 식품첨가물, 수학사, (2002).
  2. 식품의약품안전청 : 식품첨가물공전, (2008).
  3. 김명길, 윤미혜, 전일형, 김양희, 정진아 :식품 중 합성첨가물 사용실태 조사연구, 한국식품위생학회지 14(3), 244-248 (1999).
  4. 김희연, 윤혜정, 홍기형, 이창희, 박성관, 최장덕, 최우정, 박선영, 김지혜, 이철원 :식품중 인공감미료의 분석법에 관한 연구, 한국식품과학회지 36(1), 14-18 (2004).
  5. Yan zhu, Yingying Guo, Mingli Ye and Frit S. James : Separation and simultaneous determination of four artificial sweeteners in food and beverages by ion chromatography, Journal of Chromatography A, 1085, 143-146 (2005). https://doi.org/10.1016/j.chroma.2004.12.042
  6. 식품의약품안전청 :식품 중 식품첨가물분석법, (2007).
  7. Fan Ni, Jeffrey Ammann and Abudul Mabud : Moniering stevioside in Soju by high-performance liquid chromatography and liquid chromatography/mass spectrometry, Journal of AOAC International, 90(5), 1365-1372 (2007).
  8. Hiroko Matsumoto, KeikoHirata, Narue Sakamaki, Kayo Hagino and Hirofumi Ushiyama : Simultaneous determination of neotame, alitame and aspartame in foods in HPLC, Journal of the food hyginenic society of japan, 49(1), 31-36 (2008). https://doi.org/10.3358/shokueishi.49.31