Development and Validation of Analytical Methods for Picoxystrobin Determination in Agricultural Products by GC-ECD and GC-MS

Abstract

농산물 중에 있는 Picoxystrobin 잔류량을 검사하기 위해 가스크로마토그래프-전자포획검출기와 가스크로마토그래프-질량분석기를 이용한 간단하고 감도가 좋은 분석방법을 개발하였다. Picoxystrobin 잔류물은 acetonitrile 추출, 포화식염수를 이용한 액-액 분배, florisil 카트리지 정제 과정을 거쳐 기기분석을 수행하였다. 개발된 방법으로 Picoxystrobin 잔류허용기준이 설정된 식품인 고추와 사과 외 대표 농산물 시료 현미, 대두, 버섯, 감귤을 대상으로 농약을 0.02, 0.05, 0.5 mg/kg 농도로 처리하여 회수율을 시험한 결과는 64.0~98.3%이었으며, 상대표준편차는 10% 미만이었다. 검량선 작성을 위해 0.1~5 mg/L 범위로 표준품을 만들어 실험한 결과 상관계수(<TEX>$r^2$</TEX>)는 0.999로 높은 직선성을 보였으며, 분석방법의 검출한계와 정량한계는 각각 0.005와 0.02 mg/kg이었다. 또한 확인시험을 위하여 질량분석기를 사용하였으며, 145와 335를 특성이온으로 선정하였다. A simple and sensitive analytical method was developed using gas chromatography with electron capture detector (GC-ECD) and gas chromatography-mass spectrometry (GC-MS) for determination of Picoxystrobin in agricultural products (apple, hulled rice, mushroom, pepper, soybean, and mandarin). Picoxystrobin residues were extracted with acetonitrile, partitioned with saline water, and then they were cleaned up on a florisil solid-phase extraction (SPE) cartridge to obtain an extract suitable for analysis by GC-ECD and GC-MS. The method was validated using 6 agricultural product samples spiked with Picoxystrobin at different concentration levels (0.02, 0.05 and 0.5 mg/L). Average recoveries of Picoxystrobin (using each concentration three replicates) ranged 64.0~98.3% with relative standard deviations less than 10%, calibration solutions concentration in the range 0.1~5 mg/L, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.02 mg/L, respectively. The result showed that the developed analytical method is suitable for Picoxystrobin determination in agricultural products.