保健食品中有机氯农药残留分析的毛细管气相色谱条件优化  

Conditions optimization for the determination of organochlorine pesticide residues in health foods by capillary gas chromatography

作　　者：宋家玉[1] 陈金东[1] 刘文杰[1] 姜大峰[1] 焦燕妮[1] 邢金川[1] 

机构地区：[1]山东省疾病预防控制中心,山东济南250014

出　　处：《中国卫生检验杂志》2017年第22期3225-3228,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的对保健食品中有机氯农药残留量的毛细管柱气相色谱检测方法样品提取、净化和分离测定条件进行优化改进。方法样品经石油醚-丙酮(1+1,V/V)超声提取,样液经硫酸磺化、离心或凝胶净化色谱(GPC)净化,分流/不分流方式进样。采用中等极性毛细柱(DB1701、BP-608),程序升温色谱分离,电子捕获检测器检测,外标法定量。结果六六六、滴滴涕各组分在0.005μg/ml^0.10μg/ml线性关系良好,相关系数均>0.999;平均回收率为85.6%~97.9%;RSD为3.83%~7.37%(n=6);六六六总计检测限为0.003 mg/kg,滴滴涕总计检测限为0.006 mg/kg。结论经优化后的方法解决了现有国标检测方法存在的不足,操作简便、分离度高、重复性好,可满足日常保健食品中有机氯农药残留检测需要。Objective To optimize the analytical conditions of capillary gas chromatography for the determination of organochlorine pesticide residues in health foods, such as sample extraction, purification, and gas chromatographic separation.Methods The samples were extracted ultrasonically with acetone-petroleum ether（ 1 ＋ 1,V/V）. The sample solutions were sulfonated by sulfuric acid,centrifugated and purified with gel purification chromatography. The supernatants were injected with split/splitless mode. The analytes were separated with the medium polar column（ BP-608 or OV-1701） by temperature programming. The pesticide residues were detected with electron capture detector and calculated by external standard method. Results Good linearity was obtained when the concentrations of HCH and DDT were within 0. 005 μg/ml-0. 10 μg/ml,with the correlative coefficient（ r） 〉0. 999. The average recoveries ranged from 85. 6 % to 97. 9%,and the relative standard deviations（ RSDs） of 3. 83%-7. 37%（ n = 6）. The overall detection limits of HCH and DDT were 0. 003 mg/kg and 0. 006 mg/kg,respectively. Conclusion This optimal analytical method solves the deficiency of the existing GB testing methods. The method is simple and convenient to perform,and has high degree of separation with good repeatability,which is suitable for the analysis of organochlorine pesticide residues in health foods.

关 键 词：保健食品 有机氯农药残留 六六六(HCH) 滴滴涕(DDT) 毛细管气相色谱法 

分 类 号：R155.5[医药卫生—营养与食品卫生学]