气相色谱法测定贻贝中的多氯联苯和有机氯农药

Determination of Polychlorinated Biphenyls and Organochlorinated Pesticides in Mussel by Gas Chromatography

建立了贻贝中多氯联苯和有机氯农药的超声提取固相萃取净化气相色谱检测方法，以正己烷-二氯甲烷作为溶剂进行超声提取，提取液经浓硫酸溶液和硅胶-弗罗里土固相萃取柱净化，再采用GC-ECD进行分析。本方法采用外标法进行定量分析，在2.5～100μg/L浓度范围内，相关系数r2＞0.9951；多氯联苯和有机氯农药的检出限分别在0.01～0.04μg/kg和0.039～0.24μg/kg；各组分加标回收率在75％～115％之间（n＝6）， RSD＜15％。方法简便快速、重现性高，检测灵敏度和准确度均满足贻贝中多氯联苯和有机氯农药分析的要求。

A gas chromatography method was developed and validated for determination of polychlorinated biphenyls （PCBs） and organochlorinated pesticides （ OPCs） in mussel based on ultrasonic -assisted extraction and solid phase extraction as a clean-up procedure.The biological samples were extracted ultrasonically with hexane , and treated with sulfuric acid , followed by clean -up with solid phase extraction column containin octadecyl silica gel and florisil.The method realized complete base -line separation of the PCBs and OPCs and high sensitive determination based on optimization of gas chromatographic conditions , the temperature program and selected ion monitoring.Under optimizing conditions, the detection limits for PCBs and OCPs were 0.01~0.04 μg/kg and 0.039~0.24μg/kg, respectively, the calibration curves of the PCBs and OPCs were linear in the range of 2.5~100 μg/L with correlation coefficients not less than 0.995.The recoveries at the spiked amount of 1.0μg/kg, 10.0μg/kg and 100.0μg/kg were 75%~115%（ RSD〈15%）.The reproducible , sensitive and accurate method was suitable for quality control of the PCBs and OCPs in mussel.