固相萃取/毛细管气相色谱法测定肉桂皮中六六六、滴滴涕农药残留量

Determination of BHC and DDT Pesticide Residues in Cinnamomum Cassia Bark by Solid-phase Extraction and Capillary Gas Chromatography

研究了肉桂皮中六六六、滴滴涕农药残留量的测定方法.以丙酮-石油醚混合溶剂为提取剂,旋涡振荡提取,采用固相萃取技术对提取液净化,优化洗脱溶剂的比例和用量,用气相色谱/微电子捕获检测器（μECD）测定.在优化条件下,BHC及DDT农药在10～1 000 μg/L质量浓度范围内线性关系良好,相关系数为0.995 8～0.998 1.2种农药在肉桂皮中的加标回收率为92.1％～ 112％,相对标准偏差（RSD）为2.8％～8.1％,方法的检出限（LODs）为5.0×10-3～2.4×10-2mg·kg-1,定量下限（LOQs）为1.3×10-2～6.0×10-2mg· kg-1.方法具有简单、灵敏、选择性高、重现性好等优点.

A solid-phase extraction and capillary gas chromatographic method was developed for the determination of BHC ＆ DDT pesticide residues in cinnamomum cassia bark.The pesticide residues were extracted by vortex oscillation using acetone-petroleum ether mixed solvent as extraction agent,and the extract was purified by solid-phase extraction technology.The proportion and dosage of the elution solvent were optimized,and the detection of targeted compounds was performed by GC/μECD.Under the optimal conditions,the calibration curves were linear in the range of 10-1 000 μg/L,with correlations coefficients of 0.995 8-0.998 1.The average recoveries for BHC and DDT were in the range of 92.1％-112％ with RSDs （n =5） of 2.8％-8.1％.The limits of detection （LODs） were 5.0 × 10-3-2.4 × 10-2 mg· kg-1,and the limits of quantitations（LOQs） were 1.3 × 10-2-6.0 × 10-2 mg · kg-1.The method was simple,sensitive,accurate and reproducible.