안토시아닌 분석

정명근,Choung Myoung-Gun 한국작물학회 2004 한국작물학회지 Vol.49 No.suppl1

메밀 식물체 함유 Rutin의 HPLC 분석방법 개발

정명근,Choung Myoung-Gun 한국작물학회 2005 한국작물학회지 Vol.50 No.suppl1

종실에 비해 다량의 rutin이 함유된 것으로 알려진 메밀 식물체의 최적 rutin함량 분석조건을 확립하기 위해 추출조건, HPLC 분석조건, 분석 재현성 및 최소검출한계를 검토한 결과 rutin은 미황색을 나타내는 폴리페놀 성분으로 에탄올에 용해 하여 최대 흡수파장을 측정하였을 때 359nm에서 흡수 극대파장을 나타내었다. 메밀 식물체 함유 rutin의 최적 HPLC분석 조건을 검토한 결과 컬럼은 Tosoh ODS 120T를 이용하고, 검출기 파장을 355nm, 이동상으로 A용매를 $2\%$ 초산함유-$45\%$ 아세토나이트릴로, B용매는 $2\%$ 초산함유-증류수로 하여 농도구배조건을 0분 : $50\%$ A용액, 0-18분 : $100\%$ A용액, 18-20분 : $50\%$ A용액, 20-22분 : $50\%$ A용액으로 조절하고, 분당 1mL를 용출 하였을 때 가장 우수한 분리가 유도되는 것을 확인할 수 있었다. 또한 HPLC 분석요인에 대한 재현성을 검정한 결과 머무름시간, peak면적 및 peak높이의 변이 계수가 모두 $0.6\%$미만을 나타내어 극히 높은 분석 재현성을 나타내는 것으로 조사되었으며, HPLC분석 시 최소검출한계는 20ng/mL수준이었다. 메밀 식물체 함유 rutin 분석을 위한 최적 추출조건을 검토한 결과 추출용매를 에탄올로 사용하고, $80^{\circ}C$ 조건에서 120분 이상의 환류추출을 시행하는 것이 가장 바람직한 추출법으로 조사되었다. This experiment was conducted to know the appropriate methods for extraction and determination of rutin contained buckwheat plants. The efficient HPLC analytical condition of rutin contained buckwheat plants was developed. The gradient elution employed a $250mm\times4.6mm$ i.d. Tosoh ODS 120T column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of $2\%$ Acetic $acid-45\%$ Acetonitrile, and mobile phase B, comprising $2\%$ aqueous acetic acid, and delivered at a flow rate of 1mL/min as follows: 0-18 min, $50-100\%$ A; 18-20 min, $100-50\%$ A; 20-22 min, $50\%$ A. The UV detection wavelength was set at 355 nm. The limit of detection (LOD) for rutin standard compound was 20 ng/mL. And, the higher content of rutin in the extracts was obtained by $80^{\circ}C$ reflex extraction for 120 min. from plants of buckwheat using ethanol.

국내 콩 유전자원의 지방함량 및 지방산 조성변이

정명근,Choung, Myoung-Gun 한국작물학회 2006 Korean journal of crop science Vol.51 No.suppl1

고품질 콩 품종육성 및 유전자원 연구의 기초자료로 활용하기 위해 국내 콩 주요품종 46계통 및 보존 유전자원 517 계통의 지방함량과 지방산 조성의 변이양상을 분석한 결과를 요약하면 다음과 같다. 1. 한국산 콩 주요 품종의 지방함량 범위는 $15.8%{\sim}20.3%$ 였으며, 평균 18.2%를 나타내었고, 지방함량이 가장 낮은 품종은 1986년에 육성된 보광콩이, 가장 높은 품종은 2000년도에 육성된 새별콩으로 조사되었다. 2. 한국산 콩 주요 품종 46계통의 지방산 조성분석 결과 포화지방산인 C16:0 및 C18:0의 경우 각각 $8.96{\sim}13.23%$ 및 $2.55{\sim}4.20%$ 범위로 존재하였고, 불포화지방산인 C18:1, C18:2 및 C18:3의 범위는 각각 $16.33{\sim}36.41%,\;42.32{\sim}58.84%$ 및 $6.98{\sim}10.72%$를 나타내었다. 3. 국내 보존 유전자원 517계통의 지방산 조성을 분석한 결과 C16:0은 8.50%(IT 154681)${\sim}14.78%$(IT 154558), C18:0은 1.86%(IT 022331)${\sim}4.78%$(KLG 10738), C18:1은 13.29%(IT 178710)${\sim}43.30%$(IT 154657), C18:2는 38.21%(IT 156004)${\sim}61.51%$(IT 178710) 및 C18:3이 5.03(IT 188085)%${\sim}11.48%$(IT 153412)의 범위를 나타내었다. 4. 콩 함유 지방산 중 포화지방산에 속하는 C16:0 및 C18:0은 불포화지방산인 C18:1과 고도의 부의 상관을 나타내었으며, 불포화지방산인 C18:1은 다른 종류의 불포화지방산인 C18:2 및 C18:3과 고도의 부의 상관을 나타내었고, C18:2와 C18:3 사이에는 고도의 정의상관이 인정되는 것을 확인할 수 있었다. The objectives of this study was to determine the oil contents and fatty acid compositions of soybean germplasms including major Korean cultivars, and to provide the basic information of fatty acid composition for development high quality soybean varieties. Among 46 Korean major cultivated soybean samples, the oil contents were varied from 15.8% to 20.3%, and the average oil content was 18.2%. Crude oil content of cv. Saebyolkong (20.3%) was the highest among that of other cultivated soybeans. Likely many other oils of plant origin, most fatty acids in soybean are unsaturated. The highest percentage of fatty acid in soybean was linoleic acid (18:2), followed in a decreasing order by oleic (C18:1), palmitic (C16:0), linolenic (C18:3), and stearic acid (C18:0). The composition of C18:1 and C18:2 fatty acids among 563 soybean germplasms and cultivars which were positively correlated with nutritional quality of edible vegetable oil, were ranged $13.29{\sim}43.30%\;and\;38.21{\sim}61.51%$, respectively, and the C18:3 which were negatively correlated with flavor quality were varied from 5.03% to 11.48%. Also, the composition of C16:0 and C18:0 which were known to raise total cholesterol levels in human serum were ranged $8.50{\sim}14.78%\;and\;1.86{\sim}4.78%$ respectively. On the other hand, the range of fatty acid composition among 46 Korean major soybean cultivars has been investigated to be: C16:0, $8.96{\sim}13.23%$; C18:0, $2.55{\sim}4.20%$; C18:1, $16.33{\sim}36.41%$; C18:2, $42.32{\sim}58.84%$; C18:3, $6.98{\sim}10.72%$. Among the 563 germplasms tested, there are significant correlations among unsaturated fatty acids: negative between C18:1 and C18:2 (r=-0.961**) or C18:3 (r=-0.756**), and positive between C18:2 and C18:3 (r=0.608**). Also, the C18:1 was negatively correlated with saturated fatty acids, C16:0 (r=-0.231**) and C18:0 (r=-0.479**).

작약근의 오관평가와 관련된 성분 검정

정명근,Choung Myoung-Gun 한국작물학회 2005 한국작물학회지 Vol.50 No.suppl1

3년생 의성작약을 대상으로 오관검사의 평가기준으로 작용하는 맛, 색택 및 냄새에 관여하는 유리당, 유리아미노산, 유기산 및 향기성분을 분석하였다. 유리당 성분은 sucrose, glucose및 fructose등으로 구성된 것을 확인할 수 있었으며, 유리아미노산은 $\gamma-aminoisobuturic$ acid, arginine, citrulline 등 총 18종이 존재하였다. 작약근에 포함된 유기산은 oxalic acid, citric acid및 malic acid등 총 5종이 함유되어 있었다. 작약의 관능적 품질평가 기준 중 하나인 냄새를 구성하는 물질로서 eugenol을 포함한 11종의 향기성분을 확인하였다. 결국 작약의 특이적인 향기는 여러 물질에서 기인한 복합적 냄새로 평가될 수 있다. 12개정 일본 약국방 해설서(赤 등, 1991)에는 우수한 품질의 작약은 맛의 경우 처음에는 달고, 끝 맛은 떫고, 신맛이 있어야 하며, 작약의 특이한 냄새를 강하게 나타내는 것이 좋다고 기재하여 관능적 품질평가의 기준을 분명히 하였다. 그러므로 관능적 품질평가를 객관성이 결여되기 쉬운 감각적이고 주관적인 방법으로 평가할 것이 아니라 첨단 화학분석기기를 이용한 체계적 분석에 의하여 과학적이고 객관적이며 수치화된 평가방법을 적용하여 분석할 필요가 있을 것으로 판단된다. Experiment was conducted to establish the standard of quality evaluation in Korean cultivated peony roots. free sugars, free amino acids, organic acids and aromatic components, which were generally considered to be information components of five sensory test in peony roots, were examined. As free sugars, sucrose, glucose and fructose were identified in peony roots. $\gamma-aminoisobuturic$ acid, arginine and other 16 kinds of free amino acids were found in peony roots. The major organic acids of peony roots were oxalic acid, citric acid and malic acid. Eugenol and other 10 aromatic components were identified in peony roots by GC/MSD.

종실들깨와 잎들깨의 주요 특성 비교

정명근,Choung Myoung-Gun 한국작물학회 2005 한국작물학회지 Vol.50 No.suppl1

국내에서 육성된 종실용 들깨와 잎들깨 품종을 대상으로 주요특성 및 함유성분을 분석하여 용도별 들깨의 주요특성 차이를 확인한 결과를 요약하면 아래와 같다. 1. 잎들깨 품종의 평균 개화기는 9월 28일로 종실용 들깨의 평균 개화기 9월 5일보다 약 23일 늦었으며, 경장 및 마디수도 종실들깨보다 낮은 양상을 나타내어 생육상의 뚜렷한 차이를 나타내었다. 2. 종실용 들깨의 평균 천립중, 종실수량 및 기름함량이 잎들깨 품종보다 높은 양상을 나타내어 종실특성은 종실들깨가 우수하였으나, 잎 수량 및 잎 함유 안토시아닌 함량은 잎들깨 품종이 종실들깨 품종보다 각각 1.8배 및 2.1배 높은 양상을 나타내어 잎 특성은 잎들깨 품종이 우수하였다. 3. 종실용 들깨 및 잎들깨 품종의 종실 지방산 조성은 차이가 없었으며, 잎 함유 평균 엽록소 함량은 종실용 들깨가 잎들깨 품종보다 다소 높은 양상을 나타내었다. This study was conducted to know the difference of major characteristics between seed and vegetable perilla varieties. Perilla accessions examined were classified into two groups, i.e., seed perillla variety (saeyeopcildeulkkae, yangsandeulkkae, and younghodeulkkae) and vegetable perilla variety (ipdlkkae 1, namcheondeulkkae, and manbaekdeulkkae). The differences of growth characteristics were observed between two types of perilla varieties. The average flowering date of vegetable perilla varieties (Sep. 28) was 23 days later than that of seed perilla varieties (Sep. 5). Also, the stem height and node numbers of vegetable perilla varieties lower than those of seed perilla varieties. The average 1,000-seed weight, yield, and oil content of seed perilla varieties were higher than those of vegetable perilla varieties. However, as leaf characteristic, the leaf yield (1.8 times) and cyanidin content (2.1 times) were greater than in perilla variety for vegetable. No difference was observed in fatty acids composition between two types of perilla varieties. The average total chlorophyll content in leaves of seed perilla varieties was higher than in that of vegetable perilla varieties.

국내 콩 유전자원의 Isoflavone 함량 변이

정명근,강성택,한원영,백인열,김현경,신두철,강남숙,황영선,안영남,임정대,김관수,박시형,김선림,Choung, Myoung-Gun,Kang, Sung-Taeg,Han, Won-Young,Baek, In-Youl,Kim, Hyeun-Kyeung,Shin, Doo-Chull,Kang, Nam-Suk,Hwang, Young-Sun,An, Young-Nam,Lim, 한국작물학회 2006 Korean journal of crop science Vol.51 No.suppl1

고 isoflavone 함유 콩 유전자원 선발 및 품종육성의 기초자료로 활용하기 위해 국내 콩 주요품종 43계통 및 보존 유전자원 648계통의 isoflavone 함량을 분석한 결과를 요약하면 다음과 같다. 1. 한국산 콩 주요 43품종의 평균 isoflavone 함량은 daidzein이 $484.4{\pm}223.9{\mu}g/g$, genisteinol $448.0{\pm}156.2{\mu}g/g$, glyciteinol $84.9{\pm}48.7{\mu}g/g$, total isoflavoneol $1,017.3{\pm}390.0{\mu}g/g$을 나타내었다. 2. 공시된 주요 품종의 isoflavone 함량은 석양풋콩이 $2,002{\mu}g/g$으로 가장 높은 함량을 나타내었고, 황금콩이 $277{\mu}g/g$으로 가장 낮은 함량을 나타내었다. 또한 콩 주요 43품종을 용도별로 분류하여 isoflavone 함량을 비교한 결과 풋콩 및 올콩이 $1,438{\pm}493.7{\mu}g/g$을 나타내어 조사된 용도별 콩 분류 중 가장 높은 양상을 나타내었다. 3. 국내 보존 콩 유전자원 648계통을 대상으로 isoflavone 함량을 조사한 결과 IT 180001계통이 $3,479{\mu}g/g$의 함량을 나타내어 가장 높은 양상을 나타내었고, IT 910878 계통은 $82.61{\mu}g/g$의 total isoflavone을 함유하여 가장 낮은 계통으로 조사되어 보존 유전자원간에 큰 함량변이를 나타내었다. Isoflavone in soybean is known to have the important physiological functions such as antioxidative, estrogenic, and anti-tumor activities. Therefore, isoflavone content is considered as important aspect of soybean quality. The objectives of this study are to determine the isoflavone contents of soybean germplasms including major cultivars in Korea, and to provide the basic information of isoflavone far development soybean cultivar containing high isoflavone content. Among 43 Korean major cultivated soybean samples, the total isoflavone contents were varied from $277.0{\mu}g/g\;to\;2,002.0{\mu}g/g$, and the average total isoflavone content was $1,017.3{\pm}390.0{\mu}g/g$. Total isoflavone content of Seokryangputkong $(2,002{\mu}g/g)$ was the highest among those of the other cultivated soybeans. On the other side, Hwangkeumkong $(277{\mu}g/g)$ contained lower isoflavone than other cultivars. The total isoflavone content of vegetable use or early maturity soybean cultivar $(1,438{\pm}493.7{\mu}g/g)$ showed more higher total isoflavone content than others. The daidzein, glycitein, genistein and total isoflavone contents of 648 soybean germplasms collected in Korea, were ranged $16.9{\sim}2,019.8{\mu}g/g,\;0{\sim}294.9{\mu}g/g,\;38.5\sim1,337.7{\mu}g/g,\;and\;82.6{\sim}3,479.2{\mu}g/g$, respectively, and total isoflavone content of IT 180001 line $(3,479.2{\mu}g/g)$ was the highest among those of other soybean germplasm lines.

한국 콩 유전자원의 생장특성과 주요성분의 함량 비교

정명근 ( Myoung-gun Choung ),이왕희 ( Wang-hee Lee ),조병관 ( Byoung-kwan Cho ),김경환 ( Kyung-hwan Kim ) 한국환경농학회 2018 한국환경농학회 학술대회집 Vol.2018 No.-

The Korean soybean [Glycine max (L.) Merr] germplasms were categorized into four groups according to their seed coat colors, and also categorized into four groups of 100 seed weights within each seed coat color. Growth characteristics were investigated, and protein, oil, and fatty acids were determined to know the differences among the soybean germplasms, and different seed coat color and 100 seed weights. Protein contents were ranged from 43.02% to 47.70%, and average oil contents was 17.92%. Composition of oleic acids varied from 14.12% at Tongyeong-si to 29.85% at Hapcheon-gun. Average content of linoleic, and linolenic acid was 54.27% and 8.04%, respectively. Stem height, number of nodes and pods per plant, days from flower to maturity ranged from 57.3 to 182.7 cm, 13.3 to 32.7 numbers, 44.3 to 176.7 numbers, and 66.1 to 86.9 days, respectively. The 100 seed weight was negative correlated with crude protein, but a positive correlation showed between 100 seed weights and crude oil.

LC/MS를 이용한 농산물 중 Nitenpyram의 잔류분석

정명근 ( Myoung-gun Choung ),김명현 ( Myunghyun Kim ),안경근 ( Kyung-geun Ahn ),김기쁨 ( Gi-ppeum Kim ),주하은 ( Haeun Joo ),강련웅 ( Ryeon-woong Kang ),황영선 ( Young-sun Hwang ),이영득 ( Young Deuk Lee ) 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-

Nitenpyram is a neonicotinoid insecticide used in agriculture and veterinary medicine to kill external parasites of pets. This experiment was conducted to establish a determination method for nitenpyram residues in crops using LC/MS. Nitenpyram residue was extracted with acetone from representative samples of five raw products which comprised mandarin, green pepper, potato, hulled rice and soybean. The extract was evaporated and dissolved in saturated saline solution. And then the extract was washed by n-hexane partition and recovered by dichloromethane partition. The extract was finally purified by optimized Silica gel column chromatography. On an octadecylsilyl column in LC/MS, nitenpyram was successfully separated from co-extractives of sample, and sensitively quantitated by matrix-matched calibration method using selected ion monitoring(SIM) of 271.1 ion with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with nitenpyram at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 80.1 to 100.1% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of nitenpyram was 0.004 mg/kg as verified by the recovery experiment. This method using LC/MS with selected-ion monitoring technique was clearly identify the suspected residue.

축산물 중 유기인계 농약Acephate, Methamidophos 및 Monocrotophos의 잔류분석법 개발

정명근 ( Myoung-gun Choung ),주하은 ( Haeun Joo ),권희주 ( Heeju Kwon ),정주영 ( Juyoung Jeong ),김기쁨 ( Gi-ppeum Kim ),황영선 ( Young-sun Hwang ),이영득 ( Young Deuk Lee ),김정한 ( Jeong Han Kim ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-

This experiment was conducted to establish a simultaneous analytical method for 3 kinds organophosphorus pesticide in livestock products using GC-NPD/MS. All the pesticides residues were extracted with acetonitrile and/or acetone from representative samples of five livestock products which comprised beef, pork, chicken, egg and milk. The proteins in milk and egg were dispersed adding sodium oxalate, also the extract was removed non-polar co-extractives and lipids by n-hexane partition. The extract was finally purified by optimized Florisil column chromatography and NH2 cartridge. The analytes were separated and quantitated by GLC with NPD using a DB-17 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment from 5 kinds livestock product samples fortified with acephate, methamidophos and monocrotophos at 3 concentration levels in each triplication. Mean recoveries ranged from 71.9 to 113.2% in every fortification levels and compounds. The coefficients of variation were all less than 10%, irrespective of fortification levels. Limit of quantitation(LOQ) of the all analytes were 0.005 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of acephate, methamidophos and monocrotophos in livestock products.

HPLC-UVD/MS를 이용한 농산물 중 Oxycarboxin의 분석

정명근 ( Myoung-gun Choung ) 한국환경농학회 2018 한국환경농학회지 Vol.37 No.2

본 연구에서는 HPLC-UVD/MS를 이용하여 농산물 중 oxanthiin 살균제인 oxycarboxin의 잔류 분석법을 확립하였다. 대표 농산물은 현미, 콩, 배추, 고추 및 사과를 선정하였고 acetone을 가하여 추출된 oxycarboxin 성분을 dichloromethane 액-액 분배법과 Florisil 흡착크로마토그래피법으로 정제하여 HPLC-UVD/MS 분석대상 시료로 사용하였다. Oxycarboxin의 정량적 분석을 위한 최적 분석 조건을 확립하였으며, 정량한계(LOQ)는 0.04 mg/kg 이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과 모든 처리농도에서 78.3∼96.1% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 4.7%를 나타내어 잔류분석 기준인 회수율 70∼120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였으며, LC/MS SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 oxycarboxin의 HPLC-UVD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다. BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-Nphenyl- 1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ C18 column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.