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Development of a Method for Analyzing the Nicotine Content in Synthetic Flavoring Substances as Unauthorized E-cigarette Liquid by Using HPLC

전자담배 액상 충진제와 유사한 합성착향료 중 니코틴의 HPLC 분석법 개발

  • Kim, Jae-Young (Pesticide and Veterinary Drug Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Sang-Mok (Pesticide and Veterinary Drug Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chang, Moon-Ik (Pesticide and Veterinary Drug Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Cho, Yoon-Jae (Pesticide and Veterinary Drug Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Han-Jin (Pesticide and Veterinary Drug Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chae, Young-Sik (Pesticide and Veterinary Drug Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Rhee, Gyu-Sik (Pesticide and Veterinary Drug Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 김재영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이상목 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 조윤제 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이한진 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 채영식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2013.06.28
  • Accepted : 2013.10.15
  • Published : 2013.12.31

Abstract

A simple, sensitive, and specific method for quantifying the nicotine content of synthetic favoring substances (SFS) was developed using high performance liquid chromatography (HPLC) with a photo-diode array detector (PDA). Nicotine was extracted from SFS samples by using an acid-base liquid-liquid extraction method with dichloromethane and distilled water. The nicotine content was quantified by HPLC/PDA (261.9 nm) with a $C_{18}$ column under a gradient of 10% acetonitrile with 20 mM ammonium formate (ammonia solution adjusted to pH 8.7) to 100% acetonitrile. The calibration curve, analyzed from concentration standards between 0.1 to 2 mg/L, presented linearity with a correlation coefficient ($r^2$)>0.9999. The limit of quantitation (LOQ) of nicotine in SFS was 0.4 mg/kg, and the average recoveries ranged from 76.4% to 96.3%. The repeatability of measurements, expressed as the coefficient of variation (CV%), ranged from 1.74 to 5.12%. This newly developed method for nicotine quantification in SFS can be considered an analytical method with an acceptable level of sensitivity and repeatability.

전자담배는 무니코틴성이 있는 한편, 니코틴이 함유되어 있는 금연도구로서 사용된다. 전자담배의 구성품 중 액상카트리지는 식품첨가물로 사용되는 합성착향료와 유사한 성분으로 구성되어 있어, 이를 합성착향료로 사용하게 되면, 인체에 유해한 니코틴의 잔류 가능성이 존재한다. 따라서 본 연구는 식품첨가물로 사용되고 있는 합성착향료 중 니코틴 검출 분석법을 개발하였다. 분석에 사용된 검체는 시중에 사용되는 합성착향료를 이용하였다. 검체에 증류수와 디클로로메탄을 가하여 산-염기 액-액 추출법을 이용하여 추출 및 정제과정을 거친 후, 이를 질소 농축하고 이동상으로 재용해하여 HPLC/PDA에 주입하였다. 기기분석은 $C_{18}$컬럼을 사용하였고, 20 mM 개미산암모늄 함유 10% 아세토니트릴과 100% 아세토니트릴을 기울기 용리 조건으로 하여 261.9 nm에서 측정하였다. 또한, 액체크로마토그래프-질량분석기를 통해 확인시험을 수행하였으며, 모든 검증은 Codex 가이드라인의 규정에 따라 실시하였다. 그 결과, 니코틴의 정량한계는 0.4 mg/kg 수준이었고, 회수율은 76.40%-96.28%로 나타났다. 또한, 변동계수는 1.74%-5.12%로 Codex 가이드라인 규정에 만족하는 수준이었다. 따라서 개발된 분석법은 식품첨가물에 함유된 니코틴을 분석하기 위한 효율적인 분석법으로 판단된다.

Keywords

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