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HPLC-UVD/MS를 이용한 농산물 중 Oxycarboxin의 잔류분석
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 ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-
Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin fungicide is a systemic fungicide commonly used as a seed treatment to control various fungi that cause seed and seeding diseases in agronomic and horticultural crops. An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of oxycarboxin. The oxycarboxin residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and dichloromethane partition was followed to recover oxycarboxin from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Oxycarboxin was separated and quantitated by HPLC with UVD using a Zorbax SB-AQ C<sub>18</sub> column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with oxycarboxin at 3 levels per crop in each triplication. Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of oxycarboxin was 0.04 mg/kg as verified by the recovery experiment. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of oxycarboxin in agricultural commodities.
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.
국내재배 포도품종의 비타민 B₁, B₂ 및 B₃의 함량
전진수(Jinsoo Jeon),주하은(Haeun Joo),이상훈(Sang Hoon Lee),최용민(Young Min Choi),정명근(Myoung-Gun Choung) 한국식품영양과학회 2020 한국식품영양과학회지 Vol.49 No.8
한국에서 재배되는 포도 16품종에 함유된 수용성 비타민 B₁, B₂ 및 B₃의 함량을 HPLC/DAD 및 HPLC/FLD법으로 정량 분석하였다. 분석법의 재현성 검증을 위하여 조제 강화분유를 이용한 주기적 in-house quality control을 수행하였고, 분석법의 정확성 및 회수율은 표준인증물질에 대한 회수율을 확인하여 분석법의 신뢰성을 확인하였다. 한국에서 재배되는 포도 16품종에 함유된 비타민 B₁, B₂ 및 B₃의 분석 결과, 비타민 B₁은 국내 육성 품종인 ‘청수’ 품종이 0.199±0.001 ㎎/100 g을 함유하여 가장 높은 함량을 나타내었고, ‘진옥’, ‘탐나라’ 및 ‘머루포도’ 품종에서는 비타민 B₁이 검출되지 않았다. 비타민 B₂의 경우 ‘샤이니스타’(0.166±0.000 ㎎/100 g) 품종이 가장 높은 함량을 나타내었고, 총 분석된 16개의 품종 중 10품종에서 비타민 B₂가 존재하지 않음을 확인하였다. 비타민 B₃의 경우 외국 도입 품종인 ‘머루포도’(0.353±0.004 ㎎/100 g) 및 ‘캠벨얼리’(0.322±0.007 ㎎/100 g)가 높은 함량을 나타내었고, 비타민 B₂와 같은 양상으로 10품종에서는 검출되지 않았다. 한편, 수용성 비타민 B₁, B₂ 및 B₃ 성분의 함량 분석 결과를 이용하여 주성분 분석을 수행한 결과, 국내 육성 품종과 외국 도입품종은 뚜렷하게 구별되는 양상을 확인할 수 있었으며, 이 결과로 볼 때 한국에서 재배되는 포도의 수용성 비타민 B₁, B₂ 및 B₃ 성분의 함량은 품종에 따라 함량 차이가 다양함을 알 수 있다. 이 결과는 향후 한국 표준식품성분표 제10개정 출판을 위한 기초자료로 사용될 것이며, 대국민 식품 영양성분 정보 전달에 기여할 수 있을 것으로 판단된다. In this study, the content of water-soluble vitamins B1, B2, and B3 in 16 kinds of grape cultivars cultivated in Korea was analyzed by high-performance liquid chromatography/diode array detector and high-performance liquid chromatography/fluorescence detector methods. The accuracy of the analytical method was confirmed by checking the recovery for reference materials (SRM-2387 and ERM-BD600). The reproducibility of the method was assessed by performing periodic in-house quality control using fortified milk powder. An analysis of the vitamin B₁, B₂, and B₃ contents in 16 grape cultivars cultivated in Korea showed that ‘Cheongsoo’, a Korean bred cultivar, had the highest vitamin B₁ content (0.199±0.001 ㎎/100 g). In contrast, no vitamin B₁ was observed in the ‘Jinok’, ‘Tamnara’, and ‘MBA’ cultivars. ‘Shiny star’ (0.166±0.000 ㎎/100 g) had the highest vitamin B₂ content, but 10 of the 16 analyzed cultivars contained no vitamin B₂. For vitamin B₃, ‘MBA’ (0.353±0.004 ㎎/100 g) and ‘Campbell Early’ (0.322±0.007 ㎎/100 g), as introduced cultivars, showed high vitamin B3 contents, but no vitamin B₃ was detected in 10 cultivars. In principal component analysis, the Korean bred and introduced cultivars were separated on a score plot. This result shows that the vitamin B₁, B₂, and B₃ contents of grapes cultivated in Korea vary among the cultivars. This result will be used as the basic data for publication of the 10th edition of the national standard food composition table by the Korean Rural Development Administration.