毛细管气相色谱法测定三叉苦中有机氯农药残留

Determination of organochlorine pesticide residues in Melicope ptelefolia by GC

目的建立三叉苦药材中9种有机氯农药残留的毛细管气相色谱分析方法。方法将三叉苦药材粉碎后用水浸润过夜,依次用丙酮、二氯甲烷超声提取,有机层浓缩后用浓硫酸磺化净化杂质,用DB-1701弹性石英毛细管柱对待测农药组分进行分离,电子捕获检测器(ECD)进行检测。气相色谱进样口温度为230℃,ECD检测器温度为300℃,采用色谱柱升温程序(初始温度为100℃,再以10℃/min的升温速率升至220℃,接着以8℃/min的升温速率升至250℃,并保持10 min),柱流量:1.0 mL/min,不分流进样,进样量:1μL。结果该检测方法的回收率范围为73.0%～104.7%,RSD为1.3%～2.2%。结论该气相色谱分析方法快速、简便且成本低,适用于三叉苦中有机氯农药残留的检测。

Objective To establish a capillary gas chromatography （GC） method for the determination of 9 organochlofine pesticide residue in Melicope ptelefolia. Methods The sample was infilated overnight with water and extracted with acetone and dichloromethane in sequence by uhrasonography. The organic layer was condensed, then purified by concentrated sulfuric acid. DB-1701 capillary column was used. The electron capture detector （ECD） was applied to de- termine the residues of oraganochlorine pesticide. The injector temperature was set at 230℃ and the detector temperature was set at 260℃. The column temperature program was intial temperature 100℃, with the increasing rate of 10℃ per rain to 220℃, 8℃ per rain to 250℃（hold for 10 rain）. Results The average recoveries and RSD were in the range of 73.0%-104.7% and 1.3%-2.2%. Conclusion The method is rapid, simple and low in cost. It can be used for the determination of oranochlorine pesticide residues in Melicope ptelefolia.