Analytical Method Development and Monitoring of Residual Solvents in Dietary Supplements

건강기능식품 중 잔류용매 분석법 개발 및 모니터링

  • Lee, Hwa-Mi (Center for Food and Drug Inspection, Gyeongin Regional Korea Food and Drug Administration) ;
  • Shin, Ji-Eun (Center for Food and Drug Inspection, Gyeongin Regional Korea Food and Drug Administration) ;
  • Jang, Young-Mi (Center for Food and Drug Inspection, Gyeongin Regional Korea Food and Drug Administration) ;
  • Kim, Hee-Yun (Center for Food and Drug Inspection, Gyeongin Regional Korea Food and Drug Administration) ;
  • Kim, Mee-Hye (Center for Food and Drug Inspection, Gyeongin Regional Korea Food and Drug Administration)
  • 이화미 (경인지방식품의약품안전청 시험분석센터) ;
  • 신지은 (경인지방식품의약품안전청 시험분석센터) ;
  • 장영미 (경인지방식품의약품안전청 시험분석센터) ;
  • 김희연 (경인지방식품의약품안전청 시험분석센터) ;
  • 김미혜 (경인지방식품의약품안전청 시험분석센터)
  • Received : 2009.11.03
  • Accepted : 2010.03.02
  • Published : 2010.08.31

Abstract

Residual solvents in foods are defined as organic volatile chemicals used or produced in manufacturing of extracts or additives, or functional foods. The solvents are not completely eliminated by practical manufacturing techniques and they also may become contaminated by solvents from packing, transportation or storage in warehouses. Because residual solvents have no nutritional value but may be hazardous to human health, there is a need to remove them from the final products or reduce their amounts to below acceptable levels. The purpose of this study was to develop and evaluate an analytical method for the screening of residual solvents in health functional foods. Furthermore, the aim of this study was to constitute a reasonable management system based on the current state of the market and case studies of foreign countries. Eleven volatile solvents such as MeOH, EtOH, trichloroethylene and hexane were separated depending on their column properties, temp. and time using Gas Chromatography (GC). After determining the GC conditions, a sample preparation method using HSS (Head Space Sampling) was developed. From the results, a method for analyzing residual solvents in health functional foods was developed considering matrix effect and interference from the sample obtained from the solution of solvents-free health functional foods spiked with 11 standards solutions. Validation test using the developed GC/HSS/MS (Mass Spectrometry) method was followed by tests for precision, accuracy, recovery, linearity and adequate sensitivity. Finally, examination of 104 samples grouped in suits was performed by the developed HSS/GC/MS for screening the solvents. The 11 solvents were isolated from health functional foods based on vapor pressure difference, and followed by separation within 15 minutes in a single run. The limt of detection (LOD), limit of quantification (LOQ), recovery and coefficient of variation (C.V.) of these compounds determined by the HSS/GC/MS were found to be 0.1 pg/mL, 0.1-125 pg/g, 51.0-104.6%, and less than 15%, respectively. Using the developed HSS/GC/MS method, residual solvent from 16 out of 104 health functional products were detected as a EtOH. This method therefore seems t o be a valuable extension ofanalytical method for the identification of residual solvents in health functional food.

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