건강기능식품 중 잔류용매 분석법 개발 및 모니터링

이화미(Hwa-Mi Lee),신지은(Ji-Eun Shin),장영미(Young-Mi Jang),김희연(Hee-Yun Kim),김미혜(Meehye Kim) 한국식품과학회 2010 한국식품과학회지 Vol.42 No.4

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/㎖, 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.

LC-MS/MS를 이용한 한국에서 유통되는 농산물의 잔류 농약 평가

이화미(Hwa-Mi Lee),허수정(Soo Jung Hu),이현숙(Hyun-Sook Lee),박승영(Seung Young Park),김남선(Nam-Sun Kim),신용우(Yong Woo Shin),최근화(Keun Hwa Choi),김성일(Sung Il Kim),남슬이(Seul Yi Nam),조대현(Dae Hyun Cho) 한국식품과학회 2013 한국식품과학회지 Vol.45 No.4

본 연구에서 한국 유통 농산물 17품목(쌀, 사과, 배, 오렌지, 복숭아, 딸기, 바나나, 파인애플, 포도, 키위, 수박, 토마토, 오이, 호박, 참외, 깻잎, 상추 등)을 대상으로 다성분 분석농약 60종을 분석하기 위하여 대상농산물의 대분류별로 곡류에서는 현미, 두류는 메주콩, 과실류에서는 감귤, 채소류는 고추, 서류에서는 감자,버섯류에서는 느타리버섯을 선정하여 회수율 실험을 수행하였다. 60% 이상의 낮은 회수율을 나타내는 성분 중 fluquinconazole, methomyl은 4가지 이상의 농산물에서 공통적으로 낮은 회수율을 나타내었다. fluquinconazole은 식품에 적용하는 식품공전 4.1.3.22의 개별 시험법을 이용한 전처리 과정을 통해 과일류, 과채류, 콩류에서 개선된 회수율 결과를 얻을 수 있을 것으로 예상되며 methomyl 은 고추, 대두, 버섯 등 식품에 적용하는 식품공전 4.1.3.15의 개별 시험법을 통해 개선된 회수율 결과를 얻을 수 있을 것으로 예상된다. 버섯, 고추에서 공통적으로 60% 미만의 낮은 회수율을 나타내었던 butocarboxim은 현재 식품공전상 개별 시험법이 존재하지 않는 항목이므로 이에 대한 개별시험법을 개발하여 다종농약다성분 시험법을 보완할 필요가 있다고 사료된다. 한국 유통 농산물 17품목(쌀, 사과, 배, 오렌지, 복숭아, 딸기, 바나나, 파인애플, 포도, 키위, 수박, 토마토, 오이, 호박, 깻잎, 상추)을 대상으로 다성분 분석농약 60종을 분석하여 농약 잔류실태를 조사하였다. 조사대상 농산물 358건 중 대부분의 농산물인 291건(81.3%)의 농산물은 농약이 검출되지 않았으며, 67건(18.7%)의 농산물에서 농약이 검출되었으나, 잔류허용기준 미만으로 검출되었다. 쌀 등 17품목에의 다소비 농산물의 농약 잔류실태를 조사한 결과 농약의 잔류량은 잔류허용기준 미만으로 ADI 대비 EDI는 0.000009%에서 0.0861%로 위해도가 아주 낮은 것으로 조사되었으며 비교적 안전한 수준으로 농산물에 대한 농약관리가 이루어지는 것으로 판단되었다. Pesticide residues in agricultural products in Korea were evaluated to create a data base to inform food policy. Pesticide residues were investigated in 17 commodities collected from 9 provinces in 2012. Our analytical method of multiresidue analysis, involved the analysis of individual recovery, linearity, limit of detection, and limit of quantitation of 60 pesticides in six matrices. The pesticides, including acetamiprid and forchlorofenuron, were evaluated in 358 agricultural samples by liquid chromatography/tandem mass spectrometry. Twenty three pesticides were detected from 67 samples. The results showed that the ratio of estimated daily intake to acceptable daily intake was 0.00009-0.0861% by the intake assessment, which means that residual pesticides in agricultural products in Korea are properly controlled.

콘크리트 파기거동특성에 대한 실험적 연구Ⅱ

이상근(Lee, Sang-Keun),이상민(Lee, Sang-Min),이화미(Lee, Hwa-Mi),한상훈(Han, Sang-Hoon),송영철(Song, Young-Chul) 한국콘크리트학회 2003 한국콘크리트학회 학술대회 논문집 Vol.2003 No.5

LC-ESI-tandem MS를 이용한 기능성표방식품 중 부정유해물질 신속검사체계 개발

김희연(Hee-Yun Kim),이화미(Hwa-Mi Lee),장영미(Young-Mi Jang),주현진(HyunJin Joo),정용현(Young-Hyun Jung),이명숙(Myoung-Sook Lee),박종석(Jong-Seok Park),이광호(Kwang-Ho Lee) 한국식품과학회 2007 한국식품과학회지 Vol.39 No.4

부정유해물질 총 13종에 대한 신속하고 고감도의 LC-ESI-MS-MS 동시분석 방법을 개발하였으며 바데나필을 포함한 11종은 ESI positive 모드에서 타다라필을 포함한 2종은 ESI negative 모드에서 검출하는 방법으로서 시료 전처리는 간단히 메탄올 추출법을 사용하였다. 기능성표방식품 중 부정유해물질의 확인은 한번 시료를 주입함으로써 15분 이내에 13종의 분석이 가능하고 크로마토그램의 분리는 아세토니트릴과 10 mM ammonium formate가 들어있는 탈이온수를 이용한(pH 7.0) 기울기 용매 조건으로 수행하였다. 확립한 13종에 대한 부정유해물질 분석방법은 검출한계(LOD)는 0.1-5ng/㎖이고, 정량한계(LOQ)는 0.1-10ng/㎖으로서 평균 상관계수(r²)는 0.9853로서 ppb 수준에서 정량성을 가지며 회수융은 87.5-98.5%, 변동계수는 15% 이하임을 확인할 수 있었다. 또한 확립한 시험방법 LC/MS/MS를 이용하여 147건의 기능성표방식품 중의 부정유해물질의 검증을 실시한 결과, 유해 물질의 검출이 나타타지 않음을 알 수 있었다. 기능성표방식풍중의 실데나필과 그 유사물질을 포함한 13종의 부정유해물질에 대한 스크리닝 방법으로 MRM 모드를 이용한 LC-ESI-MS-MS 방법을 개발하였으며, 이는 유해물질에 대한 고성능액체크로마토그래피/자외선흡광광도법의 선택성등의 제한성을 극복한 부정유해물질의 스크리닝에 신속하고 미량까지 검출 가능한 가치 있는 방법임을 확인할 수 있었다. A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference’s characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

자연재해로 손상을 입은 지중구조물의 진단 및 보수방안

장정범(Jang Jung-Bum),송영철(Song Young-Chul),박상순(Park Sang-Soon),이상근(Lee Sang-Kuen),이화미(Lee Hwa-Mi) 한국구조물진단유지관리학회 2003 한국구조물진단학회 학술발표회논문집 Vol.- No.-

The diagnosis and rehabilitation design of a underground box structure which was seriously damaged by a natural disaster were performed in this study. The diagnosis for the damaged underground box structure includes the leveling survey, non-destructive tests and structural and soil analysis. On the basis of the diagnosis results, the structural integrity of the damaged underground box structure was evaluated and the optimal rehabilitation countermeasures were proposed. As a result, it was noticed that the structures constructed in a place where can be affected by any natural disaster has to enough consider surrounding environment at initial design stage.