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LC-MS/MS를 이용한 잔류농약 다성분 분석법의 Matrix Effect 비교
이상협 ( Sang-hyeob Lee ),곽세연 ( Se-yeon Kawk ),류준상 ( Jun-sang Ryu ),강자군 ( Ja-gun Kang ),홍성현 ( Sung-hyun Hong ),도정아 ( Jung-ah Do ),장문익 ( Moon-ick Jang ),이규식 ( Gyu-seek Rhee ),이영득 ( Young-deuk Lee ),김장억 ( 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-
This study was conducted to compare with the multi-residue analysis method for reduced a matrix effect in three agricultural products, such as orange, green pepper and brown rice. QuEChERS method involves single-phase extraction of 10 g sample with 10 mL acetonitrile. On the other hand, the improved method extracted 10 g of sample with 50 mL acetonitrile. Clean-up step used in the QuEChERS method was the d-SPE using PSA, but C18 of SPE cartridge was used for the improved method. As a result, both methods were similar in linearity and limit of quantification. The ratios that satisfy the Codex guideline were 85% of total pesticides for AOAC QuEChERS method and 88% for the improved method. Matrix effects showed different results, however, the improved method was found to produce least matrix effect. Average matrix effect QuEChERS method was -38%, and those of the improved method was -10%. Comparison of matrix effects for different agricultural products showed high variability for some residues such as dimethylthiocarbamate. It was indicated that the amount of co-extracting compounds that cause ionization suppression of pesticides depends on the agricultural products as well as on the sample preparation method employed. As a conclusion, the improved method appears to be a more suitable method because it can reduce the matrix effect rather than the QuEChERS method.
농식품 환경 분야(PF) : 국내 주요 유통 농산물 중 엽경채류에 대한 잔류농약의 통계학적 및 확률론적 분포에 따른 위해성평가
이상협 ( Sang Hyeob Lee ),전영환 ( Young Hwan Jeon ),황정인 ( Jeong In Hwang ),전상오 ( Sang Oh Jeon ),이성은 ( Sung Eun Lee ),장한섭 ( Han Sub Jang ),김장억 ( Jang Eok Kim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
최근 3년간(2010년~2012년) 국립농산물품질관리원에서 실시한 엽경채류 중 주요 유통 농산물 10종(들깻잎, 미나리, 배추, 부추, 상추, 시금치, 쑥갓, 양배추, 얼갈이배추, 열무)에 대한 농약 잔류실태조사 결과, 조사된 12,849건 중 MRL을 초과한 시료는 427건으로 부적합 시료는 0.03% 이었다. 부적합 시료 중 MRL을 초과한 농약은 acrinathrin 외 73종이었다. 엽경채류 10종 중 acrinathrin외 73종에 대한 통계학적 위해성평가를 위하여 @Risk 통계프로그램을 이용한 극단(95 percentile) 및 초극단(99 percentile) 값을 바탕으로 연령별 %ADI 및 %ARfD 평가를 실시하였다. 또한 ADI와 ARfD를 초과할 수 있는 확률론적 위해성 평가는 R 프로그램을 사용하여 Monte-Carlo simulation을 통해 수행하였다. 그 결과, 연령별 %ADI 위해도는 소아기 0.0000~0.4416%, 청소년기 0.0000~0.1486%, 성인기 0.0000~0.4276%로 나타났으며 극단값은 소아기에 최고 0.2947%, 초극단값은 소아기에 최고 0.6595%로 나타났다. 또한, 연령별 %ARfD 위해도는 소아기 0.0000~0.0074%, 청소년기 0.0000~0.0049%, 성인기 0.0001~0.0447%로 나타났으며 극단값은 소아기에 최고 0.0022%, 초극단값은 소아기에 최고 0.0961%로 나타났다. 확률론적 위해성 평가를 통해 엽경채류 중 73종 농약의 ADI 및 ARfD 초과 확률을 산출한 결과, ADI를 초과할 확률은 0.00~0.28%, ARfD를 초과할 확률은 0.05%로 극히 낮은 수준이었다. 따라서 다양한 통계학적 기법을 이용한 위해성평가 결과들로 미루어 보면 엽경채류 중 잔류농약 노출에 의한 위해성은 모두 낮은 것으로 나타났다.
GC-MS/MS를 이용한 축산물 시료 중 29종 농약의 다성분 분석법 개발
이상협 ( Sang-hyeob Lee ),곽세연 ( Se-yeon Kwak ),이동주 ( Dong-ju Lee ),허예진 ( Ye-jin Heo ),최재원 ( Jae-won Choi ),오지은 ( Ji-eun Oh ),김장억 ( Jang-eok Kim ) 한국환경농학회 2021 한국환경농학회 학술대회집 Vol.2021 No.-
The optimization and validation of multi-residue analysis for 29 pesticides in various meat matrices were evaluated. The developed method was validated in five meat matrices (pork belly, sirloin, chicken drumstick, lard, and beef tallow according to the CODEX guideline in terms of recovery, precision, calibration curve linearity, the limit of quantitation (LOQ) and matrix effect. In this study, meat samples were extracted using a QuEChERS extraction followed by optimization of sample clean-up. The clean-up method was then compared and optimized based on the d-SPE(PSA, C18, Z-SEP) and SPE cartridges(aminopropyl, C18, florisil). For the optimized analysis method, it is suitable to use the SPE cartridge as a clean-up method rather than d-SPE in order to improve the sensitivity of pesticides and reduce the matrix effect. In the clean-up method using the SPE cartridge, the use of the C18 SPE cartridge met most of the pesticide recovery criteria. The results of the optimized method showed that above 85% of pesticides gained the LOQs results of below 0.01 mg/kg, and over 90% of pesticides achieved good calibration curve linearity results (R2 > 0.99). As a result of the recovery test applied in an optimal method, more than 80% of the pesticides in the sample of pork belly, sirloin, and chicken drumstick satisfied recovery and precision criteria. In contrast, in lard and beef tallow, only 65% of pesticides met recovery and precision criteria. Therefore, it was confirmed that the recoveries measurement pesticide depends on the fat content of the samples. It can be seen that this fat content also affects a matrix effect. The average matrix effect was 16.6 ~ 30.7% in the samples of pork belly, sirloin, and chicken drumstick, while the average matrix effect was over 50% in the pork and beef fat sample. Although the matrix effect was different for each pesticide, most of the pesticides were affected by ion enhancement. In conclusion, it is judged that it will be possible to use it as a multi-residue analysis method for 29 pesticides on the meat sample.
Liquid Chromatography-Tandem Mass Spectrometry를 이용한 농산물 중 살충제 다성분 동시분석법
이상협 ( Sang-hyeob Lee ),황정인 ( Jeong-in Hwang ),강민수 ( Min-su Kang ),정혜현 ( Hye-hyun Jung ),류준상 ( Jun-sang Ryu ),홍성현 ( Sung-hyun Hong ),곽세연 ( Se-yeon Kwak ),강자군 ( Ja-gun Kang ),도정아 ( Jung-ah Do ),장문익 ( Mo 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-
For regulating pesticide residues in agricultural products imported from other countries, Korea is ready to introduce the Positive List System permitting the determination of unregistered pesticides in them at a concentration of <0.01 mg/kg. Hence, it is required to establish a rapid and sensitive analysis method for both registered and unregistered pesticides in imported agricultural products, in order to ensure their safety from pesticide residues. In this study, we developed an analytical method for 62 insecticides in three agricultural products such as orange, green pepper, and brown rice using liquid chromatography-tandem mass spectrometry. Acetonitrile and sodium citrate were used for the extraction of insecticide residues from the samples, and a dispersive solid phase extraction using primary secondary amine and anhydrous magnesium sulfate was employed for a clean-up. Using the developed method, the limits of quantification were below 0.01 mg/kg for all tested insecticides, and their matrix-matched standard calibration curve had high correlation coefficients of >0.99. In addition, for all tested samples, recoveries of insecticides fortified at levels of 0.01-0.05 mg/kg ranged from 75.2 to 111.3%, and relative standard deviations were acceptable at <18.1%. Therefore, the analytical method developed in this study could be used as the rapid and sensitive analysis method for 62 insecticides in agricultural products.
미나리, 시금치, 엇갈이배추 및 쪽파 중 살충제 Chlorantraniliprole의 잔류량 비교
조성찬 ( Sung-chan Cho ),이상협 ( Sang-hyeob Lee ),곽세연 ( Se-yeon Kwak ),홍성현 ( Seong-hyeon Hong ),김효정 ( Hyo-jeong Kim ),사커아니룻다 ( Aniruddha Sarker ),경기성 ( Kee-sung Kyung ),김태화 ( Tae-hwa Kim ),김장억 ( Jang-eok K 한국환경농학회 2018 한국환경농학회 학술대회집 Vol.2018 No.-
Different growth type of crops is one of major factors determining residual patterns of pesticides in them. In this study, residual characteristics of chlorantraniliprole in water dropworts (WD), spinach (SP), Korean cabbage (KC) and green onion (GO) which are different in leaf size and shape were investigated. Commercial chlorantraniliprole (5%, SG) was sprayed 2 times at interval of a week prior to harvest, and whole crop samples were collected at final application and harvest days. Residual amounts of chlorantraniliprole in the WD, SP, KC and GO were analyzed using HPLC-UVD, and recovery rates of chlorantraniliprole spiked with 0.4 and 2.0 mg/kg on the WD, SP, KC and GO ranged from 86.6 to 101.0%. Initial residual amounts of chlorantraniliprole were 0.51-1.26 mg/kg in WD, 0.47-2.41 mg/kg in SP, 0.32-1.86 in KC and 0.12-0.65 mg/kg in GO. These results show that initial amounts of chlorantraniliprole deposited on SP is the most amounts in four crops as opposed to GO and it may be 4 folds larger than those in GO, when assuming that weights of the SP and GO are same. Pesticides applied on SP and KC, which has wide and rough leaves, may have larger residual amount than those on WD and GO.