Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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A Study on the Analysis of Five Artificial Sweetners in Beverages by HPLC/MS/MS

HPLC/MS/MS를 이용한 음료류 중 인공감미료 동시분석에 관한 연구

  • Lee, Seong-Bong (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Yong, Kum-Chan (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Hwang, Sun-Il (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Kim, Young-Su (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Jung, You-Jung (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Seo, Mi-Young (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Lee, Chang-Hee (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Sung, Jin-Hee (Food Analysis Team, Gyeonggi-do Institute of Health and Environment) ;
  • Yoon, Mi-Hye (Food Analysis Team, Gyeonggi-do Institute of Health and Environment)
  • 이성봉 (경기도보건환경연구원 식품분석팀) ;
  • 용금찬 (경기도보건환경연구원 식품분석팀) ;
  • 황선일 (경기도보건환경연구원 식품분석팀) ;
  • 김영수 (경기도보건환경연구원 식품분석팀) ;
  • 정유정 (경기도보건환경연구원 식품분석팀) ;
  • 서미영 (경기도보건환경연구원 식품분석팀) ;
  • 이창희 (경기도보건환경연구원 식품분석팀) ;
  • 성진희 (경기도보건환경연구원 식품분석팀) ;
  • 윤미혜 (경기도보건환경연구원 식품분석팀)
  • Received : 2014.07.04
  • Accepted : 2014.10.08
  • Published : 2014.12.31
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Abstract

A method for analysis of five artificial sweetners (sodium saccharin, aspartame, acesulfame-K, sucralose, cyclamate) in beverage samples was developed using high-performance liquid chromatography/triple quadrupole mass spectrometry (HPLC/MS/MS). The method uses a single-step dilution for sample preperation. Seperation was achieved on a $C_{18}$ column ($2.1{\times}150mm$, $3.5{\mu}m$) with A- 2% methanol (1 mM ammonium acetate), B-95% methanol (1 mM ammonium acetate) as mobile phase with gradient mode. The quantitation of target compounds was performed by external calibration in selected reaction monitorning (SRM) mode. The coefficient of determination of calibration curve for sodium saccharin, aspartame, acesulfame-K, sucralose and cyclamate were 0.9957, 0.9991, 0.9943, 0.9982 and 0.9948, respectively. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.001~0.022 mg/L and 0.004~0.073 mg/L, repectively. Recoveries for beverage samples were in the range of 92.76~113.50% with RSD < 10.91%. The method has applied to the determination of the five sweetners in 102 beverage samples. Three artificial sweetners-aspartame, acesulfame-K, sucralose were detected from 42 samples. Sodium saccharin and cyclamate were not detected in all samples.

본 연구는 식품산업에서 큰 비중을 차지하고 있는 음료류에 대한 인공감미료 (삭카린나트륨, 아스파탐, 아세설팜칼륨, 수크랄로스, 싸이클라메이트)의 함유현황 파악을 위한 동시분석법을 확립하였다. 희석 및 여과의 간편하고 효율적인 전처리 후 HPLC/MS/MS를 이용하여 5종 인공감미료 동시분석 조건을 검토하였다. 컬럼은 $C_{18}$($2.1mm{\times}150mm$, 3.5 um), 이동상은 2% methanol (1 mM ammonium acetate)과 95% methanol (1 mM ammonium acetate)을 사용하여 농도구배 조건으로 각 성분을 분리하였으며 ESI/SRM 방식으로 정량 분석하였다. 0.1~5.0 mg/L의 농도범위에서 각 인공감미료 검량선은 1에 가까운 높은 직선성을 나타냈다. 검출한계, 정량한계는 각각 0.001~0.022 mg/L, 0.004~0.073 mg/L로 저농도의 감미료 분석이 가능함을 확인하였다. 회수율은 92.76~113.50%, 정밀도는 10.91% 이하로 양호하였다. 이상의 결과로 본 분석법은 음료 중 인공감미료 분석에 적합하다고 판단되었다. 확립된 분석법으로 시중 유통 중인 음료 102건 분석한 결과 42건에서 아스파탐, 아세설팜칼륨, 수크랄로스가 검출되었으며 삭카린나트륨과 싸이클라메이트는 검출되지 않았다. 검출된 인공감미료는 표시사항과 일치하였으며 사용대상과 사용량의 기준에 적합하였다.

Keywords

References

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