초록 ▼

Ⅳ. 연구개발결과
주요 농산물 중 농약의 잔류량 조사를 위해 QuEChERS 전처리법 및 LC-MS/MS를 이용한 분석법을 개발하고 회수율 실험 등으로 수행하여 검증하고자 하였으며, 상추 등 9개 작물을 대상으로 90여종의 농약의 회수율 실험결과 일부농약을 제외하고 대부분의 농약이 다성분분석적정회수율 범위(70~130%)를 나타내었으며 농산물 중 농약의 잔류량 조사 및 식이노출량 평가를 하기 위해 2012년부터 2014년까지 현지 농가를 방문하여 직접 시료를 채집 분석하였으며, 다양한 농약이 검출되었으나 검출농약의 식이섭취노출

Ⅳ. 연구개발결과
주요 농산물 중 농약의 잔류량 조사를 위해 QuEChERS 전처리법 및 LC-MS/MS를 이용한 분석법을 개발하고 회수율 실험 등으로 수행하여 검증하고자 하였으며, 상추 등 9개 작물을 대상으로 90여종의 농약의 회수율 실험결과 일부농약을 제외하고 대부분의 농약이 다성분분석적정회수율 범위(70~130%)를 나타내었으며 농산물 중 농약의 잔류량 조사 및 식이노출량 평가를 하기 위해 2012년부터 2014년까지 현지 농가를 방문하여 직접 시료를 채집 분석하였으며, 다양한 농약이 검출되었으나 검출농약의 식이섭취노출량을 분석결과 최고 0.27% 이하로써 농산물 중의 잔류농약은 안전하다고 판단되었다. 일선 안전성 분석현장에서 저비용으로 잔류농약분석을 가능하게 하기위해 가스크로마토그래피를 적용한 분석법을 설정하였고 대표적인 검출기인 ECD와 NPD를 활용하기 위해 6개 그룹 총 130종의 농약에 대한 머무름 시간과 그룹화를 추진하였으며 QuEChERS 잔류농약분석과정의 문제점인 정제과정에서 약제의 이화학적 특성에 의한 회수율 저하 문제점을 극복하기 위해 정제과정을 dispersive method가 아닌 SPE 방법을 적용하여 분석대상 약제의 고른 회수율을 나타내었음 GC 분석에서 흔하게 발생하는 matrix 효과를 상쇄하기 위해 PEG (Poly Ethylene Glycol)을 도입하였고, 이의 비교시험결과 회수율 변화에서 일부약제의 경우 회수율 증강효과를 나타내었다. 농약의 등록을 위해 제출된 자료들 중에서 12품목의 농약에 대해 모화합물 및 대사물에 대해 농산물 중 잔류농약 분석법의 검증이 실시하였다. 근채류의 원소별 평균함량은 비소 0.004∼0.008 mg/kg, 카드뮴 0.009∼0.023 mg/kg, 납은 0.116∼0.159 mg/kg으로 나타났으며, 현행기준과 대비하여 카드뮴의 경우, 0.1 mg/kg 이내로 검출되었으므로 현행기준으로 적용하여도 문제는 없으나 납의 경우, 검출 최대 농도가 0.280 mg/kg, 더덕은 0.305 mg/kg, 도라지는 0.276 mg/kg이므로 최대농도를 감안하여 0.3 mg/kg으로 기준을 설정하는 것이 타당할 것으로 판단되었다. 전국 쌀 주산단지에서 채취된 현미와 백미 각 100점에 대한 비소 분석결과 백미의 경우 평균 총비소 함량은 0.11, 무기비소는 0.07 mg/kg이었고, 현미의 경우는 각각 0.18 및 0.11 mg/kg으로 나타났다. 백미와 현미의 경우 모두 2014년에 설정된 Codex의 백미의 무기비소 기준 (0.2 mg/kg)과 2013년에 제안된 Codex의 현미 무기비소 기준안 (0.4 mg/kg)을 초과하는 시료는 없었다

Abstract ▼

This study was conducted to investigate pesticide residues in pesticide frequently detected agricultural product and to evaluate the dietary exposure about the detected pesticide. In order to the analysis of pesticide residues of the agricultural products, pesticide residues analysis method using wi

This study was conducted to investigate pesticide residues in pesticide frequently detected agricultural product and to evaluate the dietary exposure about the detected pesticide. In order to the analysis of pesticide residues of the agricultural products, pesticide residues analysis method using with QuEChERS sample preparation and LC-MS/MS was developed and validated. Recovery experiments of 90 pesticides on nine crops such as lettuce were carried out. the results showed the recoveries of most of the pesticides were satisfied with multi-residue analysis appropriate recovery range 70 to 130%. These showed the analysis method using with QuEChERS sample preparation and LC-MS/MS could be applied to monitoring of pesticide residues in 9 crop. To the investigation and dietary exposure assessment of pesticide residues in agricultural products, crop samples were directly collected form local farm in main producing area from 2012 to 2014. lettuce, leek, spinach, chainese cabbage, radish, and perilla leaf were collected and analyzed in 2012. and Aster scaber, leek, strawberry, cucumber, and perilla leaf were collected and analyzed in 2013 to 2014. As results of pesticide residual analysis of collected crop samples, 4 to 43 kinds of pesticides were detected, and some of them were exceeded maximum residue limits. However, the dietary exposure of detected pesticides in each crop was estimated on basis of acceptable dailey intake(ADI) of pesticides. and this results was below maximum 0.27% and it showed that pesticide residues in 9 crop was safe. For exposure assessment of residual pesticides in agricultural products, Simultaneous analysis method of several pesticide using LC-MS/MS targeted at leaf vegetables was developed. And this method’s informations such as analysis instrument condition and recoveries of pesticides was provided to analyst in regional agricultural research institutes. Purification methods with various SPE kit depends on sample character were settled and distributed to local inspection institute. Each analytical methods forfluopyram, epoxiconazole, pyribencab, flutianil, pyraclonil and valifenalate in agricultural commodities were developed. Those pesticides were in the progress of being registered in Korea for the first time and therefore the efficient analytical methods were needed to establish MRLs(maximum residue limits) and detect those pesticides in various commodities. The developed methods include solvent extraction, liquid-liquid partition and florisl column chromatography, and solid phase extracton(SPE) were used in some cases. Each steps of analytical method were optimized for each pesticides. The instrumental conditions were tested for quantitation in GC and HPLC and for confirmation in GC/MS and LC/MS/MS. Recoveries of all pesticides were in the range of 70~120% with RSD≤20% and the quantitation limits(LOQ) of method were 0.01~0.05mg/kg in all samples. The results showed that the developed methods can be applied to residue analysis of pesticides in agricultural commodities. Analysis of heavy metal exposure in agri-food and risk assessment were conducted to estimate dietary exposure of heavy metals from crops and to evaluate the risk. Hazardous heavy metal(loid) content and dietary exposure for some vegetables and rice were investigated for As, Cd and Pb. Mean lead content in ginseng, deodeok and ballon flower was much higher (0.116-0.159 mg/kg) than other root vegetables, so new food standard higher than 0.3 mg/kg was suggested. For Chinese chive, the lead content was higher and so reassessment was also suggested. Mean As content in polished rice was 0.07 mg/kg and no sample was observed exceeding CODEX standard (0.2 mg/kg). Risk from the consumption of these vegetables and rice was minor comparing to the PTWI for each hazardous element. For the vegetablesstudied in this research, bioconcentration factor (BCF) was calculated. The BCF was dependent on the element and type of crop. The BCFs of As and Cd were higher than EPA values for root vegetables. For Pb, the BCF of root vegetables was also higher than BCFs used in the UK and the Netherlands.