School of Chemical and Biological Engineering, University of Science and Technology Beijing, Beijing, People's Republic of China.
Bull Environ Contam Toxicol. 2011 Apr;86(4):444-8. doi: 10.1007/s00128-011-0224-0. Epub 2011 Feb 18.
A simple analysis method to detect clomazone residues in soybean and soil was developed using solid phase extraction coupled with high performance liquid chromatography with diode-array detection. The pesticide residues present in soybean and soil matrices were extracted with methanol-water and extracts purified with Florisil cartridges. The analytes from soybean and soil matrix were eluted with petroleum ether-acetic ether (10 mL, 95:5, v/v) and petroleum ether-acetic ether (2 mL, 95:5, v/v), respectively. The overall recovery of fortified soybean and soil at the levels of 0.01, 0.1 and 0.5 mg/kg ranged from 89.75% to 106.6%, and the coefficients of variation (CV) ranged from 1.68% to 4.93% (n = 3). The limit of quantification (LOQ) is 0.01 mg/kg. This method has been applied to the analysis of clomazone in real samples of soybean and soil. The dissipation of residue over the time in soil coincided with C = 1.189e(-0.0926t ) and the half-lives (T(1/2)) was 7.48 days. The final residue in soybean was lower than 0.01 mg/kg at harvest time. Direct confirmation of the analyte in real samples was achieved by gas chromatography-mass spectrometry.
建立了一种使用固相萃取结合高效液相色谱二极管阵列检测检测大豆和土壤中氯甲唑残留的简单分析方法。采用甲醇-水提取大豆和土壤基质中的农药残留，用 Florisil 小柱对提取物进行纯化。用石油醚-乙酸乙酯（10 mL，95:5，v/v）和石油醚-乙酸乙酯（2 mL，95:5，v/v）分别洗脱大豆和土壤基质中的分析物。在 0.01、0.1 和 0.5 mg/kg 加标水平下，大豆和土壤的总回收率为 89.75%至 106.6%，变异系数（CV）为 1.68%至 4.93%（n = 3）。定量限（LOQ）为 0.01 mg/kg。该方法已应用于实际大豆和土壤样品中氯甲唑的分析。土壤中残留量随时间的消散符合 C = 1.189e(-0.0926t)，半衰期（T(1/2)）为 7.48 天。收获时大豆中的最终残留量低于 0.01 mg/kg。通过气相色谱-质谱法直接确认了实际样品中的分析物。
