高效液相色谱法检测蔬菜中百菌清及其代谢产物的方法研究

Determination of chlorothalonil and its metabolite residues in vegetables by HPLC

建立了同时检测蔬菜中百菌清(CHT)及其代谢产物(4-羟基百菌清,CHT-OH)残留的高效液相色谱分析法。样品经丙酮提取,弗洛里硅土柱净化浓缩后以适量甲醇定容,HPLC紫外检测器检测,以C18色谱柱分离,甲醇∶水(90∶10,V/V)为流动相,流速为0.7mL/min,检测波长240nm。结果表明,百菌清、4-羟基百菌清的检测线性范围分别为0.05～10mg/kg和0.01～10mg/kg,相关系数r=0.9999。方法检出限分别为0.012mg/kg和0.005mg/kg,二者的平均加标回收率为83.5%～121.3%,RSD为2.4%～4.6%,该方法可用于市售蔬菜样品的测定。

The high performance liquid chromatography （HPLC）method for the simultaneous detection of chlorothalonil and its metabolite（4-hydroxyl chlorothalonil）residues in vegetables was established.Residues were extracted from vegatables with acetone contained 1.6% phosphate,cleaned up by Flory silica, and separated on a C18 column （250mm × 4.6mm i.d. ,5μm） using methanol-water formate （90：10, by volume） as mobile phase at a flow rate of 0.7mL/min.The detection wavelength was set at 240rim.The results showed that the linear range of detection of chlorothalonil and 4-hydroxyl chlorothalonil were from 0.05mg/kg to 10mg/kg and from 0.01 mg/kg to 10mg/kg, respectively.Standard curve correlation coefficient （r）both were 0.9999.The detection limit of chlorothalonil was 0.012mg/kg and 4-hydroxyl chlorothalonil was 0.005mg/kg.The average recovery ranged from 83.5% to 121.3%, and the RSD was from 2.4% to 4.6%.The method was successfully used for commercial vegetable samples.