土壤样品有机氯农药残留GC/MS测定方法的优化

近年来土壤样品中有机氯农药的测定需求迅速增加. 参考国内外测定方法，按照实验室批量测定实际样品的要求，从消除背景干扰、提高测定数据质量出发，对样品前处理和仪器分析的各环节进行了系统的试验研究，全面优化了有机氯农药的GC/MS测定方法. 采用严格的质量保证/质量控制措施，包括对进样口滴滴涕分解的控制、合理选择有机氯农药定性和定量离子、使用有证标准样品进行验证试验等. 22种有机氯农药的清洁基体加标回收率为70%～110%，方法检出限为0.032 5～0.445 0 ng/g. 

Optimization of the Determination Method for Organochlorine Pesticide Residues in Soil Samples by GC/MS

The demand for organochlorine pesticide (OCP) determination in soil samples has been increasing rapidly in recent years. According to the previous standard methods and the requirements of laboratory measurement for batch samples, systematic experimental studies were carried out on each step of the sample pretreatment and instrumental analysis starting from eliminating background interference and improving data quality. Therefore, the analytical method of OCPs in soils by GC/MS was comprehensively optimized. All analytical procedures were monitored using strict quality assurance and quality control measures including control of inlet degradation of DDT, sound selection of qualitative and quantitative ions for OCPs, and the usage of Standard Reference Materials. The results suggest that recoveries of the 22 OCPs on the clean matrix spiked test ranged from 70% to 110%, and the method detection limits ranged from 0.0325 to 0.4450 ng/g.