自制新型液相色谱柱同时测定土壤中两种农药

用自制的新型N-苄氧羰基-(-)-L-苯甘氨酰-(-)-L-苯甘氨酰基键合硅胶液相色谱固定相(简称BCPGPG色谱固定相)在正相条件下对土壤中氰戊聚酯和氯氰菊酯两种农药进行了分析与测定,建立了可同时测定土壤中的氰戊菊酯和氯氰菊酯含量的正相高效液相色谱方法。样品用流动相(正己烷/二氯甲烷=8/1,V/V)溶解,过滤,然后以BCPGPG固定相柱进行色谱分离,在254nm处进行测定。结果表明,氰戊菊酯和氯氰菊酯的质量浓度为0～2.0mg/L时其峰面积与质量浓度的线形关系良好;批间(n=4)测定的平均相对偏差(RSD)分别为5.70%和5.5%;回收率分别为81.0%～96%和88.0%～96.7%。该方法适合于测定氰戊聚酯和氯氰菊酯两种农药的含量测定,方法准确,操作简便。

Simultaneous Determination of Two Kinds of Agricultural Chemicals in Soil by a New Amino Acid-derived Stationary Phase for HPLC

By N-Benzyloxycarbonyl-L-Phenylglycine-L-Phenylglycine-derived Silica Gel Stationary Phase(BCPGPGSP),a simple and reliable positive-phase high performance liquid chromatographic (HPLC) method for the routine analysis of cypermethrin and fenvalerate in soil has been established. HPLC determination for the sample was performed in a BCPGPGSP column and detected at 254nm. Using a mixed solvent of hexane-dichloromethane(80～10, V/V) as the mobile phase, and the flow rate was 1.0mL/min.The method was proved to be liner in the ranges of 0～2.0mg/L for cypermethrin and fenvalerate. The relative standard deviations of inter-assay (n=4) were 5.70% for cypermethrin analysis and 5.5% for fenvalerate analysis. The recoveries of cypermethrin and fenvalerate were 81.0%～96% and 88.0%～96.7% respectively. The method has been successfully applied to the simultaneous determination of the cypermethrin and fenvalerate in soil.