摘要
目的：建立气相色谱-电子捕获检测器法(GC-ECD)测定大米中六六六和滴滴涕(α-六六六、β-六六六、γ-六六六、δ-六六六、o,p’-滴滴滴、o,p’-滴滴伊、o,p’-滴滴涕、p,p’-滴滴滴、p,p’-滴滴伊、p,p’-滴滴涕)残留量的方法。方法大米样品经乙腈超声提取后,应用PSA进行分散固相萃取净化,高速离心后氮吹浓缩定容,最后使用气相色谱电子捕获检测器测定。结果六六六和滴滴涕在0.002~0.1 mg/L 浓度范围内呈现良好线性关系, R2大于0.99；在0.002、0.005、0.01 mg/kg三个添加浓度上回收率范围为84.10%~111.43%,相对标准偏差小于9.23%,检出限在0.0001~0.0007 mg/kg之间。结论该方法前处理操作快速简单,重复性好且灵敏度高,满足国内外对大米中六六六和滴滴涕快速、准确检测的要求,可应用于大量样品的定性定量分析。
Objective To develop a method for the simultaneous determination of hexachlorocyclohexane (HCH) and dichlorodiphenyltrichloroethane (DDT) (α-HCH, β-HCH, γ-HCH, δ-HCH, o,p’-DDD, o,p’-DDE, o,p’-DDT, p,p’-DDD, p,p’-DDE, p,p’-DDT) residues in rice by gas chromatography with ECD detector using dispersive solid phase extraction. Methods Rice samples were extracted with acetonitrile assisted by ul-tra-sonic, and the extracts were purified by dispersive solid phase extraction using PSA as the purification sor-bent. After high speed centrifugation and concentrated by nitrogen flushing, samples were detected by GC-ECD. Results The method showed a good linearity in the range of 0.002~0.1 mg/L for HCH and DDT with R2>0.99. The recoveries were in the range of 84.10%~111.43% at three spiked levels of 0.002, 0.005, 0.01 mg/kg for HCH and DDT, and the relative standard deviations (RSDs) were less than 9.23%. The limits of detections were in the range of 0.0001~0.0007 mg/kg. Conclusion The method is suitable for quantitative and qualita-tive analysis of HCH and DDT in a sufficient number of rice samples with sensitivity and repeatability, and which could meet the fast and accurate detection requirements of HCH and DDT residues testing at home and abroad.
出处
《食品安全质量检测学报》
CAS
2014年第4期1117-1124,共8页
Journal of Food Safety and Quality
基金
中粮集团公司资助项目(2012-C2-F013)~~
关键词
六六六
滴滴涕
分散固相萃取
气相色谱法
大米
hexachlorocyclohexane
dichlorodiphenyltrichloroethane
dispersive solid phase extraction
gas chromatography
rice
