Analysis of Four Pesticides, Isoproturon, Phenmedipham, Pyridate and Nitenpyram Residues by High-Performance Liquid Chromatography with Diode-Array Detector

A method for the determination of four pesticide compounds, urea (isoproturon), bis-carbamate (phenmedipham), thiocarbamate (pyridate) and vinyllidenediamine (nitenpyram) were examined and analyzed by HPLC with C-18 column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size). Mobile phase consisted of deionized water, acetonitrile and 50 mM $KH_2PO_4$ (pH 2.5). Isoproturon and phenmedipham analytical condition was isocratic elution of the column with 50% solvent A (acetonitrile) and 50% solvent B (deionized water); pyridate was 85% solvent A (acetonitrile) and 15% solvent B (deionized water) at a flow rate of 1 mL/min; and nitenpyram analytical condition was 90% solvent A (50 mM $KH_2PO_4$, pH 2.5) and 10% solvent B (acetonitrile) at a flow rate of 1 mL/min. In results, retention times were 6.12, 8.63, 9.40 and 12.76 min for isoproturon, phenmedipham, pyridate and nitenpyram, respectively. All injection volumes were $10\;{\mu}L$ and the limit of quantitation was 0.05 mg/kg for four pesticide compounds, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four pesticide compounds were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 70.18% to 118.08% and the standard deviations of all experiments were within 10%.

HPLC를 이용한 Isoproturon, Phenmedipham, Pyridate 및 Nitenpyram 4종 성분의 잔류농약 분석법 개발

Bis-carbamate계(phenmedipham), urea계(isoproturon), thiocarbamate계(pyridate) 및 vinyllidenediamine계(nitenlyram) 4종의 농약을 HPLC를 이용하여 분석하는 방법을 개발하였다. 사용된 칼럼은 C-18($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size)이며 isoproturon, phenmedipham은 acetonitrile과 물을 50:50으로 섞어서 사용하였으며, pyridate는 acetonitrile과 물을 85:15로, nitenpyram은 phosphoric acid를 이용하여 pH 2.5로 맞춘 50 mM $KH_2PO_4$와 acetonitrile을 90:10으로 섞어 유속 1 mL/min의 isocratic 조건으로 분석하였다. 시료 주입량은 $10\;{\mu}L$이며 retention time은 isoproturon 6.12분, phenmedipham 8.63분, pyridate 9.40분, nitenpyram 12.76분, 정량한계는 모두 0.05 mg/kg이었다. 회수율 실험은 쌀, 사과 및 대두에 4종의 농약 표준품을 각각 0.05, 0.1 및 0.5 mg/kg이 되도록 세 가지 농도로 spiking 하였으며, 회수율 및 분석오차는 70.18~118.08% 범위와 10% 이내를 만족하였다.