earticle

영어

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 to be a valuable extension of analytical method for the identification of residual solvents in health functional food.

한국어

본 연구에서 용매 총 11종에 대한 HSS/GC/MS 분석 방법을 개발하였다. 확립한 용매 11종에 대한 HSS/GC/MS 잔류용매 분석 방법은 검출한계(LOD)는 0.1 pg/g이고, 정량범위는 0.1-125 pg/g으
로서 평균 상관계수(R2)는 0.9961로서 ppm수준에서 정량성을 가지며, 회수율은 51.0-104.6%, 변동계수는 15%이하임을 확인 할 수 있었다. 또한, 확립한 시험방법 HSS/GC/MS를 이용하여 104건의 건강기능식품 중의 잔류용매 검증을 실시한 결과, 주정의 경우 에탄올로서 18건이 검출되었고, 그 외는 검출되지 않았다.
건강기능식품 중의 주정과 같은 용매를 포함한 11종의 잔류용매에 대한 분석 방법으로 HSS/GC/MS 방법을 개발하였고, 이 방법은 잔류용매에 대한 분석법의 확대와 잔류용매 실태관리를 위한 가치있는 방법이라고 사료된다. 건강기능식품 중 잔류용매의 신속 검사체계 방법을 확립하였으며, 이 검사방법은 ppm level의 미량 성분까지도 분석이 가능하였다. 또한, 이 검사 방법은 정량성이 확보된 분석 방법으로서, 공정시험법의 제개정 자료로 활용될 수 있을 것으로 기대된다.