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Proficiency Testing for the Gas-chromatographic Analysis of Procymidone, Chlorpyrifos and Metolachlor Residues in Soil

가스크로마토그래피를 이용한 토양 중 프로사이미돈과 클로르피리포스, 메톨라클로르의 잔류분석 숙련도시험

  • Kim, Chan-Sub (Department of Agro-Food Safety, National Academy of Agricultural Science, Rural Development Administration) ;
  • Son, Kyeong-Ae (Department of Agro-Food Safety, National Academy of Agricultural Science, Rural Development Administration) ;
  • Gil, Geun-Hwan (Department of Agro-Food Safety, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kim, Jin-Bae (Department of Agro-Food Safety, National Academy of Agricultural Science, Rural Development Administration) ;
  • Hong, Su-Myeong (Department of Agro-Food Safety, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kwon, Hye-Young (Department of Agro-Food Safety, National Academy of Agricultural Science, Rural Development Administration)
  • 김찬섭 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 손경애 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 길근환 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김진배 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 홍수명 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 권혜영 (농촌진흥청 국립농업과학원 농산물안전성부)
  • Received : 2012.12.06
  • Accepted : 2013.03.26
  • Published : 2013.08.30

Abstract

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On October 2011 the testing was carried out using the soil collected and kept as the moistened state for five years, which is expected to very low residue levels of pesticides. The soil was fortified with chlorpyrifos, metolachlor and procymidone in a manner similar to prepare soil sample for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soil treated as different levels, one of which was used to the assesment and another used to confirm. In addition, provide three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty seven institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of chlorpyrifos and procymidone were 44, metolachlor 40.

농약등록 잔류시험 연구기관의 측정 능력 향상 및 신뢰도 향상을 위해 잔류분석 숙련도 시험을 실시하였다. 시험은 2011년 10월에 토양시료를 사용하여 수행되었다. 토양은 채취 후 습토상태로 5년간 보관하여 농약의 잔류수준이 매우 낮을 것으로 기대되는 밭토양을 사용하였다. Chlorpyrifos와 metolachlor, procymidone을 토양잔류시험의 실내시험 토양시료 조제방법과 유사하게 처리하여 분배 포장하였고, 그 중 일부를 임의로 선정하여 시료의 균질도와 상온에서의 안정성을 확인하였다. 시험참여기관마다 3종 농약이 두 수준으로 처리된 토양시료 2점을 배분하였는데 그 중 하나는 모든 기관에 동일한 농도로 처리된 평가용이었고, 기관별로 다른 농도의 시료는 확인용으로 사용하였다. 아울러 대상농약성분의 정량을 방해하는 성분의 확인과 회수율시험 등에 사용할 수 있도록 무처리 토양과 3종 농약의 표준용액(농도 10 mg/L)을 제공하였다. 대상기관 중 47개 기관이 결과를 제출하였고 제출된 분석결과의 중앙값을 잔류농약에 대한 설정값으로 사용하였다. 합목적(fitness-for purpose) 표준편차는 토양잔류시험의 변이계수 허용한계 20%를 적용하여 계산하였다. 개별성분에 대한 평가에는 Z-score를 적용하였고, 3종 농약에 대한 전체적인 평가는 Z-score의 절대값의 평균으로 하였다. Z-score의 절대값이 2 이하로 적합하다고 평가된 기관은 chlorpyrifos와 procymidone의 경우 44개, metolachlor는 40개 기관이었다. 따라서 본 숙련도시험결과 잔류시험 연구기관 대부분의 잔류분석 수행능력은 적절한 것으로 판단되었다.

Acknowledgement

Grant : 농약시험 연구기관 정도관리체계 확립

Supported by : 농촌진흥청

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