固相萃取-毛细管气相色谱法测定莪术中15种有机氯农药的残留量

Determination of organochlorine pesticide residues in Curcuma phaeocaulis by solid-phase extraction and capillary gas chromatography

目的用固相萃取-毛细管气相色谱分析方法测定莪术中15种有机氯农药残留量。方法样品以混合溶剂超声提取、Florisil固相萃取小柱净化处理后，采用DB-1701毛细管气相色谱柱分离样品，电子捕获检测器检测。内标法定量，计算有机氯农药的残留量。结果15种农药在5～500μg·L^-1范围内具有良好的线性关系，相关系数均大于0．995。15种农药3个不同浓度的平均回收率为83．1％～110．6％，RSD％为3．4％～14．8％。最小检测量为0．08～1．5μg·L^-1被测样品中均含有不同程度的有机氯农药。结论本法简便、灵敏、准确、重现性好，可用于中药材中有机氯类农药的残留量测定。

Objective To establish solid-phase extraction and capillary gas chromatography for the determining 15 organochlorine pesticide residues（OCPs） in Curcuma phaeocaulis. Methods The 15 organochlorine pesticides were extracted from samples with solvents by ultrasonic and cleaned up by Florisil solid-phase extraction column . Then, the extract was separated by capillary column and detected by electron capture detector. The internal standard method was used for quantitative determination. Results There was good liner relation over the range of 5-500μg· L^- 1. The average recoveries and RSD were in the range of 83.1-110.6% and 3.4-14.8% at three spiked mixed organochlorine pesticides levels, respectively. The limits of detection were 0.08- 1.5 μg · L^-1. Organochlorine pesticide residues were detected in all samples. Conclusion This method is effective, fast, accurate, repeatable and suitable for analysis organochlorine pesticide residues in tradition Chinese medicines.