생물훈증제 개발을 위한 국내 자생식물의 선발

김희연(Hee-Yun Kim),최해진(Hae-Jin Choi),허수정(Su-Jeong Heo),임상현(Sang-Hyun Lim),김경희(Kyung-Hee Kim),이유선(Yu-Sun Lee),김미성(Mi-Sung Kim),김성문(Songmun Kim) 한국원예학회 2005 한국원예학회 학술발표요지 Vol.2005 No.5

국내산 녹차의 잔류농약 모니터링

김희연(Hee-Yun Kim),전종섭(Jong-Sup Jeon),김용훈(Yong-Hoon Kim),최희주(Hee-Ju Choi),정소영(So-Young Cheong),이화정(Hwa-Jeong Lee),김재인(Jae-In Kim),김영선(Young-Seon Kim),최계선(Gye-Sun Choi),최재천(Jae-Chun Choi) 한국식품과학회 2009 한국식품과학회지 Vol.41 No.5

국내유통 녹차 100품목 중 조사대상 61종 농약의 잔류실태를 조사한 본 연구의 결과는 다음과 같다. 총 100품목의 시료 가운데 22품목의 시료에서 bifenthrin, chlorpyrifos, dicofol, EPN, chlorfenapyr, tebuconazole, cyhalothrin, difenoconazole 및 tebufenpyrad 등 9종의 농약이 검출되었다. bifenthrin이 1개 품목(검출치: 0.12 ppm, 기준: 0.3 ppm), chlorpyrifos가 3개 품목(검출치: 0.24-0.78 ppm, 기준: 2.0 ppm), dicofol이 2개 품목(검출치: 1.64-4.19 ppm, 기준: 50.0 ppm), EPN이 1개 품목(검출치: 0.13 ppm, 기준: 0.05 ppm), chlorfenapyr가 16개 품목(검출치: 0.01-1.23 ppm, 기준: 3.0 ppm), tebuconazole이 1개 품목(검출치: 0.71 ppm, 기준: 5.0 ppm), cyhalothrin이 5개 품목(검출치: 0.05-0.3 ppm, 기준: 2.0 ppm), difenoconazole이 1개 품목(검출치: 0.23 ppm, 기준: 2.0 ppm), tebufenpyrad가 2개 품목(검출치: 0.06-0.07 ppm, 기준: 2.0 ppm)이었고 이 가운데 2종 이상의 잔류농약이 검출된 것은 7개 품목이었다. 기준치를 초과한 것은 EPN(검출치: 0.13 ppm, 기준: 0.05 ppm) 1종이었고 나머지는 기준치 이하를 보여주었다. 검출 품목의 지역별 분포는 보성산이 5품목, 제주가 14품목이었고, 기타 국내산이 3품목이었다. 검출 품목의 제품유형별 농약 검출수와 종 수는 잎차(leaf green teas)의 경우 우전이 3품목, 1종, 세작이 2품목, 1종, 중작이 3품목, 2종 및 대작이 1품목, 1종이었고 가루녹차(milled green teas)의 경우는 5품목, 6종, 티백(green tea bag)의 경우는 8품목, 6종 이었다. 농약 종 수와 검출율에 있어 가루녹차와 티백이 잎차보다 훨씬 큰 것으로 나타났는바 가루녹차와 티백이 일반 국민이 다소비하는 품목이라는 점에서 중점관리가 필요하다 할 것이다. 녹차에 잔류하는 농약의 잔류수준은 EPN을 제외하고는 비교적 안전한 수준으로 인체에 크게 위협이 되지 않는 수준인 것으로 판단되었다. 검출 농약 중 dicofol과 EPN은 차류의 잔류농약허용기준에 포함되지 않은 농약으로서 향후 관리가 필요한 것으로 사료된다. Herein, we present the results of our investigation of 61 pesticide residues in 100 samples of green teas obtained from Korean markets. Bifenthrin, chlorpyrifos, dicofol, EPN, chlorfenapyr, tebuconazole, cyhalothrin, difenoconazole, and tebufenpyrad were detected in 22 of the 100 green tea samples. The quantity of pesticide residues for bifenthrin was 0.12 ppm (maximum residue limits (MRLs): 0.3 ppm) in one sample, chlorpyrifos was 0.24-0.78 ppm (MRLs: 2.0 ppm) in three samples, dicofol was 1.64-4.19 ppm (MRLs: 50.0 ppm) in two samples, EPN was 0.13 ppm (MRLs: 0.05 ppm) in one sample, chlorfenapyr was 0.01-1.23 ppm (MRLs: 3.0 ppm) in 16 samples, tebuconazole was 0.71 ppm (MRLs: 5.0 ppm) in one sample, cyhalothrin was 0.05-0.3 ppm (MRLs: 2.0 ppm) in five samples, difenoconazole was 0.23 ppm (MRLs: 2.0 ppm) in one sample, and tebufenpyrad was 0.06-0.07 ppm (MRLs: 2.0 ppm) in two samples. More than two pesticide residues were detected in seven samples. All detected pesticide residues (with the exception of EPN) were within the MRLs.

HPLC-UVD를 이용한 농산물 중 스피노사드 분석법 개선 및 잔류실태 조사

김희연(Hee Yun Kim),최선희(Sun Hee Choi),정소영(So Young Chung),최희주(Hee Ju Choi),김용훈(Yong Hoon Kim),조민자(Min Ja Cho),서은채(Eun Chae Seo),한경진(Kyoung Jin Han,),최재천(Jae Chun Choi),박희옥(Hee Ok Park),하상철(Sang Chul Ha) 한국식품과학회 2011 한국식품과학회지 Vol.43 No.2

본 연구는 단성분 농약 중 스피노사드의 잔류실태를 조사하기 위하여 식품공전의 스피노사드 분석법을 농산물에 적용되도록 개선하고 개선된 시험법으로 잔류실태조사가 부족한 스피노사드에 대한 잔류실태를 조사하였다. 국내 유통 중인 16종의 농산물 304건에 대한 스피노사드 잔류량을 조사한 결과 모든 검체에서 검량한계 이상 검출 되지 않았다. 스피노사드 시험법의 회수율은 현미, 강낭콩, 오렌지, 들깻잎, 표고버섯에서 스피노사드 A의 경우 0.05 mg/kg 수준에 각각 76.2, 95.3, 83.5, 79.9, 98.6%이고, 0.25 mg/kg 수준에 각각 97.3, 86.6, 84.4, 94.0, 88.1%이고, 스피노사드 D의 경우 0.05 mg/kg 수준에 각각 76.6, 104.0, 88.9, 74.9, 81.1%이고, 0.25 mg/kg 수준에 각각 92.7, 97.7, 86.9, 90.4, 85.4%였으며 검출한계 0.001 mg/kg, 검량한계 0.005 mg/kg이다. 회수율에 대한 모든 표준편차는 10% 미만이다. 스피노사드 A와 D는 0.1-5.0 mg/kg 범위에서 상관계수(r<SUP>2</SUP>) 0.9999 이상의 높은 직선성을 보이고, 검출한계는 0.001 mg/kg, 검량한계는 0.005 mg/kg이었다. The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient (r<SUP>2</SUP>) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

고시의약품 시험에 사용되는 유해시약 대체 시험법 개발

김희연(Hee Yun Kim),강현경(Hyun Kyung Kang),최선희(Seon Hee Choi),방수진(Su Jin Bang),한경진(Kyung Jin Han),최승희(Sung Hee Choi),김진희(Jin Hee Kim),이화정(Hwa Jung Lee),강찬순(Chan Soon Kang) 大韓藥學會 2010 약학회지 Vol.54 No.2

Development of alternative testing methods for the replacement of hazardous reagents with less hazardous ones is strongly enforced because exposure of human and environment to hazardous reagents are restricted and hazardous reagents are gradually prohibited from using in various testing methods. Thus, in this study, we developed 8 monographs from the Korean Pharmaceutical Codex by substituting the use of the hazardous reagents including ICH class 1 such as benzene, chloroform and dioxane to the use of less toxic ones like ICH class 2 or 3 reagents. We also improved their qualification and quantification performance. Among 8 monographs, the 6 newly developed TLC methods for the identification of nifedipine, oxolamine citrate, ketoprofen lysinate, chlorquinaldol, retinol acetate, and riboflavin showed a clear spot of corresponding material without any interference in spite of the replacement with ICH class 2 or 3 reagents. For the quantification of domperidone and trimebutine, HPLC methods were developed for the substitution of UV/VIS spectrometry and titrimetry, respectively. These HPLC methods were validated for the linearity, recovery, reproducibility, and inter-laboratory variations. In conclusion, the newly developed methods could be expected to become valuable tools for revising the Korean Pharmaceutical Codex.

식품첨가물중 불용성광물성물질의 물리화학적 특성

김희연(Hee-Yun Kim),이영자(Young-Ja Lee),홍기형(Ki-Hyoung Hong),권용관(Yong-Kwan Kwon),김소희(So-hee Kim),김현종(Hyun-Jong Kim),이철원(Chul-Won Lee),김길생(Kil-Saeng Kim),이상훈(Sang-Hoon Lee) 한국식품과학회 1999 한국식품과학회지 Vol.31 No.5

고시 수재 의약품의 용출규격 설정 - 구연산니카메테이트 정, 노르플록사신 캡슐

김희연(Hee Yun Kim),최선희(Seon Hee Choi),방수진(Su Jin Bang),한경진(Kyung Jin Han),최승희(Sung Hee Choi),백지윤(Ji Yun Baek),김동섭(Dong Sup Kim),김영옥(Young Ok Kim),손경희(Kyung Hee Sohn),송영미(Young Me Song),사홍기(Hong Kee Sah) 大韓藥學會 2010 약학회지 Vol.54 No.5

Despite the fact that the dissolution test can serve as an effective tool for drug quality control and prediction of in vivo drug performance, there are a number of drugs with no established dissolution specifications because they were developed quite a long time ago. Under this circumstances, KFDA started the new project that establishes dissolution method and specifications for drugs with no dissolution specifications listed in the Korea Pharmaceutical Codex (KPC). This project aims for promoting the appropriate management of oral solid dosage forms. Seoul regional KFDA selected 2 items, Nicametate citrate tablet and Norfloxacin capsule, for establishing dissolution specifications. We went through the following procedures to develop the dissolution method and specifications: (1) Validation of dissolution test equipment, (2) Purchase of test drugs, (3) Preliminary test with one of the test products (1 lot), (4) Validation of analysis methods (3 lots), (5) Final tests and cross tests among other laboratory to establish dissolution specifications, (6) Additional test with the other test drugs. The outcome of this study will be reflected in revision of the KPC. It is believed that the quality control and evaluation of oral solid dosage forms listed in KPC will be advanced with the revision which adds additional dissolution test and specifications for the drugs with no established dissolution specifications.

식품 중 아목시실린, 암피실린, 옥소린산 및 플루메퀸의 분석

김희연(Hee-Yun Kim),최희주(Hee-Ju Choi),김용훈(Yong-Hoon Kim),최선희(Sun-Hee Choi),정소영(So-Young Cheong),이화정(Hwa-Jeong Lee),김재인(Jae-In Kim),최계선(Gye-Sun Choi),최재천(Jae-Chun Choi) 한국식품과학회 2009 한국식품과학회지 Vol.41 No.5

본 연구에서 확립한 분석법으로 총 393건의 시료를 분석한 결과 넙치에서 아목시실린 9건, 장어에서 옥소린산 4건과 플루메퀸 1건이 검출되었다. 아목시실린의 검출농도는 0.009-0.078 mg/kg의 범위를 나타내었고, 옥소린산의 검출농도는 0.02-0.20 mg/kg의 범위를 나타내었다. 플루메퀸은 잔류허용기준(0.5 mg/kg) 이하의 농도로 장어 1건(0.03 mg/kg)에서 검출되었다. The present study was performed to validate an analytical method for veterinary drugs, including amoxicillin, ampicillin, oxolinic acid and flumequin, in meat, fish, and their products as established in the 2007 Korea Food Code, and to monitor the respective drugs in 6 kinds of foods, namely beef, pork, flatfish, rockfish, freshwater eel and shrimp. Additionally, an HPLC-ESI-MS/MS method was developed for the qualification of these veterinary drugs. As a result of monitoring, these drugs were detected in 14 (3.6%) out of 393 samples. In particular, amoxicillin was detected in 9 flatfish samples, and oxolinic acid and flumequin were detected in 4 samples and 1 sample of freshwater eel, respectively. The detection levels of amoxicillin ranged from 0.009 to 0.078 mg/kg, in which 1 sample of flatfish contained more than the MRL (0.05 mg/kg). Flumequin detected in 1 sample of freshwater eel, was less than the MRL (0.5 mg/kg). Therefore, the majority of detected levels were less than the MRLs, with the exception of 2 samples showing amounts that were 1-2 times higher than the MRLs. The detected veterinary drugs were identified and confirmed by the HPLC-ESI-MS/MS method created in this study.

유통 중인 어류의 중금속 모니터링

김희연(Hee-Yun Kim),김진철(Jin-Chul Kim),김서영(Seo-Young Kim),이진하(Jin-Ha Lee),장영미(Young-Mi Jang),이명숙(Myoung-Sook Lee),박종석(Jong-Seok Park),이광호(Kwang-Ho Lee) 한국식품과학회 2007 한국식품과학회지 Vol.39 No.4

본 연구는 우리나라에서 유통되고 있는 어류를 전국 10개 연안지역에서 수거된 해산어류 35종 531건과, 전국 내륙지방 및 주요도시에서 수거된 담수어 12종 80건을 대상으로 납, 카드뮴, 비소, 구리, 망간, 아연, 총수은 함량을 분석하였다. 전처리방법(습식분해법, 변형된 microwave 분해법, microwave 분해법)에 따른 각각의 분해조건을 비교ㆍ검토한 결과, microwave 분해법이 회수율이 가장 우수한 것으로 확인되었다. ICP-MS를 이용하여 수은을 제외한 6종 금속의 회수율을 측정한 결과 약 94-108%를 보였으며, mercury analyzer를 이용한 수은의 회수율은 99%를 나타냈다. 해산어류 중 중금속 평균 함량은 비소 2.523, 카드뮴 0.017, 구리 0.569, 납 0.023, 수은 0.068, 망간 0.395 및 아연 6.086 ㎎/㎏으로 나타났다. 담수어 중 중금속 평균함량은 비소 0.370, 카드뮴 0.011, 구리 0.628, 납 0.026, 수은 0.058, 망간 1.150 및 아연 9.980 ㎎/㎏으로 나타났다. 우리나라에서 유통 중인 어류에서 섭취되는 중금속 함량을 FAO/WHO에서 설정된 잠정주간섭취허용량인 PTWI와 비교한 결과 카드뮴, 수은, 납이 각각 0.9, 1.6 및 0.9%로 나타나 조사된 어류를 통한 우리나라 국민들의 중금속섭취는 현재까지는 안전한 수준인 것으로 판단된다. This survey was carried out to estimate the heavy metal contents of fishes (531 ocean fishes and 80 freshwater fishes) sold in and around Korea from April to October in 2006. The contents of arsenic (As), cadmium (Cd), copper (Cu), lead (Pb), manganese (Mn), zinc (Zn) and mercury (Hg) were estimated by inductively coupled plasma-mass spectrometry (ICP-MS) and a mercury analyzer. The concentrations [mean (minimum-maximum) ㎎/㎏] of heavy metals in the ocean fishes were as follows: As=2.523 (0.140-65.543), Cd=0.017 (0.000-0.108), Cu=0.569 (0.040-5.634), Pb=0.023 (0.000-0.323), Hg=0.068 (0.002-0.754), Mn=0.395 (0.016-4.651) and Zn=6.086 (0.529-34.729). The concentrations of heavy metals in the freshwater fishes were: As=0.370 (0.024-2.231), Cd=0.011 (ND-0.086), Cu=0.628 (0.003-1.962), Pb=0.026 (ND-0.423), Hg=0.058 (0.006-0.349), Mn=1.150 (0.069-7.230) and Zn=9.980 (3.463-82.737). The weekly intakes of Cd, Hg and Pb from fish were 0.9, 1.6 and 0.9%, respectively, as compared with the Provisional Tolerable Weekly Intake (PTWI) established by Joint FAO/WHO Expert Committee for food safety evaluation.

국내 유통 중인 농산물의 중금속 함량 모니터링

김희연(Hee-Yun Kim),김재인(Jae-In Kim),김진철(Jin-Chul Kim),박지은(Ji-Eun Park),이경진(Kyung-Jin Lee),김성일(Sung-Il Kim),오재호(Jae-Ho Oh),장영미(Young-Mi Jang) 한국식품과학회 2009 한국식품과학회지 Vol.41 No.3

본 연구는 식품공전의 농산물 중금속 기준규격 설정으로 인한 사후 관리 차원에서 유통 중인 농산물 10품목에 대하여 중금속 함량을 조사하였다. 전국에서 유통 중인 다소비 농산물 쌀, 옥수수, 대두, 팥, 감자, 고구마, 배추, 무, 시금치, 파 421건을 2007년 4월부터 10월까지 구입하고 중금속 4종(As, Cd, Pb, Hg)을 수은 분석기 및 ICP-MS를 이용하여 분석하였다. 시료의 분해는 microwave법을 이용하였으며 분석 장비로 사용된 ICP-MS 및 수은분석기의 검출한계와 정량한계는 각각 0.002-0.025 μg/kg 및 0.023μg/kg로 높은 감도를 나타내었다. 10품목의 농산물에 대한 중금속 4종의 분석결과는 다음과 같다. 납의 평균값은 쌀 0.021, 옥수수 0.020, 대두 0.028, 팥 0.034, 고구마 0.025, 감자 0.021, 배추 0.019, 시금치 0.031, 파 0.021, 무 0.011 mg/kg으로 나타났고 카드뮴은 쌀 0.021, 옥수수 0.002, 대두 0.020, 팥 0.006, 고구마 0.008, 감자 0.011, 배추 0.007, 시금치 0.035, 파 0.006, 무 0.006mg/kg, 비소는 쌀 0.103, 옥수수 0.005, 대두 0.007, 팥 0.005, 고구마 0.005, 감자 0.004, 배추 0.007, 시금치 0.0152, 파 0.009, 무 0.006 mg/kg, 수은은 쌀 2.3, 옥수수 0.2, 대두 0.6, 팥 1.4, 고구마 0.1, 감자 0.3, 배추 0.5, 시금치 2.1, 파 0.5, 무 0.2 μg/kg의 결과를 보였다. 2006년에 설정된 기준규격에 대해 초과한 것은 한 건도 없었다. 또한 2005년 국민영양조사 결과보고서의 1일 섭취량을 근거로 FAO/WHO의 중금속 잠정주간섭취허용량과 비교하면 Pb, Cd 및 Hg은 각각 2.6, 8.7, 및 1.2% 수준으로 식이를 통한 안전에는 문제가 없는 것으로 판단된다. This survey was conducted as a surveillance program following the establishment of safety guidelines for agricultural products in Korea. Concentrations of arsenic (As), cadmium (Cd), lead (Pb), and mercury (Hg) were measured in 421 samples using a mercury analyzer or ICP-MS. The average levels of Pb in mg/kg were 0.021 for rice, 0.020 for corn, 0.028 for soybeans, 0.034 for red beans, 0.025 for sweet potatoes, 0.021 for potatoes, 0.019 for Chinese cabbage, 0.031 for spinach, 0.021 for Welsh onions, and 0.011 for radishes. The average levels of Cd in mg/kg were 0.021 for rice, 0.002 for corn, 0.020 for soybeans, 0.006 for red beans, 0.008 for sweet potatoes, 0.011 for potatoes, 0.007 for Chinese cabbage, 0.035 for spinach, 0.006 for Welsh onions, and, 0.006 for radishes. The average levels of As in mg/kg were 0.103 for rice, 0.005 for corn, 0.007 for soybeans, 0.005 for red beans, 0.005 for sweet potatoes, 0.004 for potatoes, 0.007 for Chinese cabbage, 0.015 for spinach, 0.009 for Welsh onions and, 0.006 for radishes. Finally, the average levels of Hg in μg/kg were 2.3 for rice, 0.2 for corn, 0.6 for soybeans, 1.4 for red beans, 0.1 for sweet potatoes, 0.3 for potatoes, 0.5 Chinese cabbage, 2.1 for spinach, 0.5 for Welsh onions, and 0.2 for radishes. Based on the Korean public nutrition report 2005, these levels (or amounts) are calculated only at 2.6% for Pb, 8.7% for Cd, 1.2% for Hg of those presented in provisional tolerable weekly intake (PTWI) which has been established by FAO/WHO. Therefore, the levels presented here are presumed to be adequately safe.

식품 중 프로필렌글리콜의 분석법 개발

김희연(Hee-Yun Kim),홍기형(Ki-Hyoung Hong),최장덕(Jang-Duck Choi),박성관(Sung-Kwan Park),정시섭(Si-Sub Jung),최우정(Woo-Jeong Choi),이신호(Shin-Ho Lee),문동철(Dong-Chul Moon) 한국식품과학회 2005 한국식품과학회지 Vol.37 No.6