Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Analysis of sorbic acid in tea-drink using isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS)

동위원소희석 액체 크로마토그래피-질량분석법을 이용한 차음료 중의 소르빈산의 분석

  • Ahn, Seong-Hee (Division of Metrology for Quality Life, Korea Research Institute of Standards and Science) ;
  • Lee, In-Sun (Dong-il SHIMAZU Corp. R&D center) ;
  • Kim, Byung-Joo (Division of Metrology for Quality Life, Korea Research Institute of Standards and Science)
  • 안성희 (한국표준과학연구원 삶의질 표준부) ;
  • 이인선 (동일 시마즈) ;
  • 김병주 (한국표준과학연구원 삶의질 표준부)
  • Received : 2011.12.29
  • Accepted : 2012.01.18
  • Published : 2012.02.25
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Abstract

Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

동위원소희석 액체크로마토그래피-탄뎀질량분석법을 이용하여 차음료 중의 소르빈산을 정밀하게 측정하는 방법을 개발하였다. 소르빈산의 동위원소, $^{13}C_2$-소르빈산은 주문합성하여 구입하였다. 질량 분석기는 음이온 모드로 선택반응분석법 (Selected Reaction Monitoring mode)에서 수행하여, $[M-H]^-$ 이온이 $[M-CO_2H]^-$ 조각이온으로 가는 m/z 111 ${\rightarrow}$ 67와 $^{13}C_2$-소르빈산 m/z 113 ${\rightarrow}$ 68 채널을 선택하여 분석하였다. 분리는 C18 컬럼으로 수행되었으며, 암모니움 아세테이트용액(pH 4.5) 55%와 메탄올 45%로 이동상을 구성하였다. 반복성과 재현성을 포함한 방법의 유효성 검토를 위하여 본 연구원에서 차음료에 소르빈산을 강화하여 균질성있는 기준물질을 제조하였다. 반복성과 재현성 결과는 동위원소희석 액체크로마토그래피-탄뎀질량분석법에 의한 소르빈산의 분석이 신뢰할만 하며 재현성 있는 방법임을 보여주었고, 기준물질들의 소르빈산의 농도는 3.8%의 표준편차를 보여주었다.

Keywords

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