A rapid determination method of BHC and DDT residues in rice husk had been developed by triple tandem quadrupole GC-MS. Or-ganic phase was extracted by methylene chloride, then purified by automatic solid-phase extraction apparatus, and further condensed by ro-tavapor. After the separation by DB-1701 capillary column, MS was performed by using selective ion detection mode which could identify the ratio of ion abundance to determine its chemical formula, and internal standard method was used to quantitate. Within mass concentration of 4~160 ppb, BHC and DDT had good linear relationships (correlation coefficient were greater than 0.99), and the detection limit was 0.10~2.15 ppb. With two addition levels of BHC and DDT in rice husk, the recovery rates of BHC and DDT varied from 84.2%to 109.7%, and its RSD was between 4.3%and 7.4%. The method was accurate and reliable, and it was suitable for qualitative and quantitative analysis of BHC and DDT residues in rice husk.%采用三重串联四级杆气质联用仪建立了稻壳中六六六和滴滴涕农药残留的快速检测方法.采用乙腈提取,经全自动固相萃取仪净化,旋转蒸发仪浓缩;经DB-1701毛细管柱分离后进行质谱分析,采用选择性离子检测模式,以子离子丰度比定性,内标法定量.六六六与滴滴涕在4~160 ppb质量浓度范围内线性关系良好(相关系数均大于0.99),方法检出限为0.10~2.15 ppb.稻壳中六六六与滴滴涕的两个添加水平的回收率在84.2%~109.7%,重复性的相对标准偏差(RSD)在4.3%~7.4%之间.该方法准确可靠,适用于稻壳中六六六与滴滴涕农药残留的定性定量分析.
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