超声萃取-高效液相色谱分析法测定土壤中2-氯-6-(三氯甲基)吡啶

Determination of Nitrapyrin in Soil by Ultrasonic Extraction and High Performance Liquid Chromatography

用Agilent SB-C18(150 mm×4.6 mm,5.0μm)色谱柱,在优化流动相最佳体积比和流速的条件下,用超声萃取-高效液相色谱法测定不同类型土壤中硝化抑制剂--2-氯-6-(三氯甲基)吡啶(nitrapyrin,CP)的质量浓度.结果表明:土壤样品经3次乙醇溶剂超声萃取后,通过有机滤膜净化,以V(乙腈)∶V(水)=4为流动相,在0.8 mL/min流速下10 min内完成色谱柱(Agilent SB-C18)的分离,提取效果较好;在0~75 mg/L内,CP的质量浓度与峰面积呈显著的线性关系(R^2=0.9998,p<0.01);空白土壤中CP的检出限为0.42 mg/L;不同质量浓度和剂型的CP溶液在草甸黑土、黑钙土和风沙土中添加24 h后的回收率为82.44%~91.66%,标准偏差为1.34~5.04,变异系数为0.02~0.06.

Ultrasonic extraction-high performance liquid chromatography was adopted to determinate the mass concentration of nitrification inhibitor-nitrapyrin in different soil types using the Agilent SB-C18(150 mm×4.6 mm,5.0μm)chromatographic column under the condition of optimizing the best volume ratio and the flow rate of the mobile phase.The results show that the best extracting effect is that the soil sample is disposed by the organic solution of ethanol for three times continuously followed by organic filter membrane to purify,then chromatographic column of Agilent SB-C18 is separated under the condition of the mobile phase being V(acetonitrile)∶V(water)=4,and completing within 10 min at the flow rate of 0.8 mL/min.There is a significant linear relationship between the mass concentration of nitrapyrin and the peak area in the range of 0-75 mg/L(R^2=0.9998,p<0.01).The detection limit of nitrapyrin in blank soil is 0.42 mg/L.The recovery rate of nitrapyrin for different mass concentrations and dosage forms in meadow black soil,chernoze and aeolian soil is 82.44%-91.66%after 24 h of addition with the standard deviation of 1.34-5.04 and the coefficient variation of 0.02-0.06.