Department of Chemistry, University of Mazandaran, Babolsar, Iran.
J Sep Sci. 2010 Apr;33(8):1044-51. doi: 10.1002/jssc.200900494.
A comparison between C(18) silica and multi-walled carbon nanotubes (MWCNTs) in the extraction of Chlorpyrifos and Phosalone in environmental water samples was carried out using HPLC. Parameters affecting the extraction were type and volume of elution solvent, pH and flow rate of sample through the adsorbent. The optimum conditions obtained by C(18) cartridge for adsorption of these pesticides were 4 mL dichloromethane as elution solvent, sample pH of 5, flow rate of 1 mL/min, and those for MWCNT cartridge were 3 mL dichloromethane, pH of 5 and flow rate of 10 mL/min, respectively. Optimized mobile phase for separation and determination of these compounds by HPLC was methanol/water (80:20 v/v) with pH=5 (adjusted with phosphate buffer). Under optimal chromatographic and SPE conditions, LOD, linear range and precision (RSD n=8) were 3.03x10(-3), 0.01-5.00 microg/mL and 2.7% for Chlorpyrifos and 4.03x10(-4), 0.01-5.00 microg/mL and 2.3% for Phosalone, in C(18) cartridge, respectively. These values for MWCNT were 4.02x10(-6), 0.001-0.500 microg/mL and 1.8% for Chlorpyrifos and 1.02x10(-6), 0.001-0.500 microg/mL and 1.5% for Phosalone, respectively.
使用高效液相色谱法对 C(18) 硅胶和多壁碳纳米管 (MWCNTs) 在环境水样中萃取毒死蜱和 phosalone 的性能进行了比较。影响萃取的参数有洗脱溶剂的类型和体积、pH 值以及样品通过吸附剂的流速。C(18) 柱吸附这些农药的最佳条件为 4 mL 二氯甲烷作为洗脱溶剂、样品 pH 值为 5、流速为 1 mL/min，MWCNT 柱的最佳条件分别为 3 mL 二氯甲烷、pH 值为 5 和流速为 10 mL/min。优化的 HPLC 分离和测定这些化合物的流动相为甲醇/水 (80:20 v/v)，pH=5(用磷酸盐缓冲液调节)。在最佳色谱和 SPE 条件下，C(18) 柱对毒死蜱的检测限、线性范围和精密度 (RSD n=8)分别为 3.03x10(-3)、0.01-5.00 microg/mL 和 2.7%，对 phosalone 的检测限、线性范围和精密度分别为 4.03x10(-4)、0.01-5.00 microg/mL 和 2.3%。MWCNT 对毒死蜱的检测限、线性范围和精密度分别为 4.02x10(-6)、0.001-0.500 microg/mL 和 1.8%，对 phosalone 的检测限、线性范围和精密度分别为 1.02x10(-6)、0.001-0.500 microg/mL 和 1.5%。
