气相色谱-质谱法测定贝类样品中的有机氯农药

Determination of organochlorine pesticides in shellfish samples by GC-MS

建立气相色谱质谱法测定贝类样品中10种有机氯农药(包括六氯苯、α-六六六、β-六六六、γ-六六六、δ-六六六、七氯、p,p′-DDE、o,p′-DDT、p,p′-DDD、p,p′-DDT)含量的分析方法。样品经高速组织匀浆机匀浆后采用正己烷振荡提取、自制酸性硅胶柱净化,内标法定量分析。10种有机氯农药在5.0~250.0μg/L范围内线性相关性良好,相关系数均在0.99以上;方法检出限为0.1~1.6μg/kg;方法准确度高、可靠性好,低、中、高不同浓度水平样品的加标回收率为62.3%~118%(n=7),相对标准偏差(RSD)为1.1%~21%。应用该方法对实际样品扇贝和花蛤进行分析,加标回收率在61.5%~120%之间,结果满意。

A method for the determination of 10 organochlorine pesticides in shellfish, includingHexachlorobenzen, a-BHC, β-BHC, γ-BHC, δ-BHC, Heptachlor, p, p＇-DDE, O, p＇-DDT,p, p＇-DDD and p, p＇-DDT, was proposed. Tested samples were homogeneousl mixing by high-speed tissue homogenate and extracted by Hexane, and then cleaned up by home-made acidicsilie gel column, thus determined by GC-MS. The results showed that the liner ranges for 10organoehlorine pesticides were 5.0-250.0 μg/L, the linear dependence was good, with thecorrelation coefficients all above 0.99. The proposed method is accurate, reliable and sensitive.The method detection limits （MDLs） wererecoveries were between 62.3 %- 118% （n=7）,21%. The method was applied to analysisspiked recoveries were between 61.5%-120%.in the range of 0.1-1.6 μg/kg, and the spikedthe relative standards （RSDs） were between 1.1%-of real samples including scallop and astarte, the