毛细管气相色谱法测定白芍中有机氯农药的含量

Determination organochlorine pesticide residues in paeonia lactiflra pall by capillary-gas chromatography

在建立白芍中七氯、环氧七氯及滴滴涕异构体含量的气相色谱分析方法中,样品以石油醚加丙酮在索氏提取器中提取,提取液以浓硫酸净化;采用DB-5(30 m×0.25 mm×0.25 μm)弹性石英毛细管柱分离样品;以GC-ECD检测农药七氯、环氧七氯及滴滴涕的含量(色谱条件:载气为N2(99.999%,1.5 mL/min);分流比为2.3∶1;进样器温度为200 ℃,检测器测试为330 ℃,柱升温程序是从100 ℃(保持0.5 min)开始以15 ℃/min升至200 ℃保持1.0 min),再以4 ℃/min升至240 ℃(保持7 min);方法的加标平均回收率为96.27%～100.3%,精密度为2.0%～6.9%.

The capillary GC method was introduced for determination of HEPT and HCE and DDT in paeonia lactiflra pall. The HEPT and HCE and DDT were extracted from soil and platycodon grandiflorum with mixed solvents （petroleum ether＋ acetone） ,cleaned up by concentrated sulfuric acid,separated by capillary column,and detected by ECD. The capillary column was DB-5 （30 m）〈 0. 25 mm）〈 0.25μm ）; carrier gas N2 （99. 999 %, 1.5 mL/min） ; split ratio 2.3 ：1; injector temperature 200℃ ; detector temperature 330 ℃; column temperature program 100℃ （hold 0. 5 min）, rate of 15 ℃· min%-1 to 200℃ （hold 1.0 min）, rate of 4℃·min^-1 to 240℃（hold 7 min）. The average recoveries were within 96. 27%～100.3% and RSD 2.0～6.9%.