School of Chemical and Biological Engineering, University of Science & Technology Beijing, Beijing, China.
J Environ Sci Health B. 2012;47(5):385-9. doi: 10.1080/03601234.2012.648533.
A simple and efficient residue analysis method for direct determination of ioxynil octanoate in maize and soil was developed and validated with High Performance Liquid Chromatography-Ultra Violet (HPLC-UV). The samples were extracted with mixtures of acetonitrile and deionized water followed by Solid Phase Extraction (SPE) to remove co-extractives prior to analysis by HPLC-UV. The recoveries of ioxynil octanoate extracted from maize and soil samples ranged from 86 %-104 % and 84 %-96 %, respectively, with relative standard deviation (RSD) less than 7.84% and sensitivity of 0.01 mg kg(-1). The method was applied to determine the residue of ioxynil octanoate in maize and soil samples from experimental field. Data had shown that the dissipation rate in soil was described as pseudo-first-order kinetics and the half-life (t(1/2)) was less than 1.78 days. No ioxynil octanoate residue (<0.01 mg kg(-1)) was detected in maize at harvest time withholding period of 60 days after treatments of the pesticide. Direct confirmation of the analytes in field trial samples was realized by Liquid Chromatography-Mass Spectrometry (LC-MS).
建立并验证了一种高效、简便的残留分析方法,采用高效液相色谱-紫外检测(HPLC-UV)法直接测定玉米和土壤中辛酰碘苯腈的残留量。样品经乙腈-去离子水混合溶液提取,固相萃取(SPE)净化后,采用 HPLC-UV 进行分析。辛酰碘苯腈在玉米和土壤中的平均回收率为 86%-104%和 84%-96%,相对标准偏差(RSD)小于 7.84%,检测限为 0.01mg/kg。该方法应用于田间试验玉米和土壤样品中辛酰碘苯腈残留量的检测。结果表明,辛酰碘苯腈在土壤中的消解符合一级动力学方程,半衰期(t(1/2))小于 1.78 天。施药 60 天后收获时,玉米中的辛酰碘苯腈残留量低于检测限(<0.01mg/kg)。采用液相色谱-质谱法(LC-MS)对田间试验样品中的目标物进行了直接确证。