Development and Validation of Analytical Method for Determination of Imidacloprid Residues in/on Soil and Water by HPLC Abstract A rapid, sensitive and reliable HPLC method was developed for the determination of imidacloprid residue in different pH of water and soil. The Validation of analytical method for determination of imidacloprid residues by HPLC. The method consisted of extracting with methanol from soil. The extracts were subjected onto the column filled with florisil column chromatography. The extraction of imidacloprid residues from water with ethyl acetate. Quantification is performed by reversed phase HPLC with UV detector. The limit of quantitation (LOQ) was mg/kg 0.02 in soil and 0.02 mg/L in water. The limit of detection (LOD) was 0.01 mg/kg in soil and 0.01mg/L in water. Recoveries for imidacloprid were 95.18, 94.66, 95.27 and 94.78 % in black, red, sandy loam and clay soil respectively. Recoveries for imidacloprid were 96.86, 86.14, and 92.34 % in pH4, pH7, and pH9 respectively. The detector linearity and the repeatability of the method proved to be very precise. 全文可以在线浏览： http://www.eco-web.com/editorial/03588.html
Determination of imidacloprid in water and soil samples by gas chromatography-mass spectrometry J. L. Vilchez et,al. Journal of Chromatography A Volume 746, Issue 2, 11 October 1996, Pages 289-294 Abstract: A method for determination of imidacloprid in water and soil samples, previous hydrolysis in basic medium, followed by gas chromatography-mass spectrometry and selected ion monitoring. A 250-ml sample water was previously heated in basic medium to give a hydrolysis compound of adequate volatility. The hydrolysis product which was extracted and isolated with chloroform was identified and found to be suitable for gas chromatography analysis. Further, a clean-up is not necessary using the selected ion monitoring mode. [2H10]Anthracene was used as an internal standard. The applicable concentration range was 5–20 μg l−1. Detection limit was 0.16 μg l−1 for water and 1 μg kg−1 for soil samples. Their relative standard deviations established for different concentration levels were between 0.3 and 1%. It was applied to the check whether there was imidacloprid above these limits on waters and soil from Granada (Spain). The method was validated applying the standard addition methodology. Recovery levels of the method reached 100% in all cases.
Simultaneous determination of imidacloprid, thiacloprid, and thiamethoxam in soil and water by high-performance liquid chromatography with diode-array detection YING Guang-Guo Abstract A high-performance liquid chromatography method with diode-array detection (HPLC-DAD) is described for the determination of three neonicotinoid insecticides imidacloprid. thiacloprid, and thiamethoxam in soil and water. The soil samples were extracted with acetonitrile, while the water samples were extracted using C18 cartridges. The mean recoveries plus standard deviations for spiked soil samples were 82±4.2% for thiamethoxam. 99±4.2% for imidacloprid and 94 ± 1.4% for thiacloprid. The recoveries for water samples ranged from 87±3.4% for thiamethoxam to 97 ±3.9% for imidacloprid and 97±2.6% for thiacloprid. The limits of quantitation (LOQ) were 0.1, 0.1, 0.01 mg/kg in soil (5g), and 2, 2, 11.5 μg/L in water (50 mL) for thiamethoxam, imidacloprid, and thiacloprid, respectively.
Journal of environmental science and health. Part B. Pesticides, food contaminants, and agricultural wastes；2004, vol. 39, no5-6, pp. 737-746 [10 page(s) (article)] (12 ref.)
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