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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 and improve the extraction, purification and separation conditions for the determination of organochlorine pesticide residues in health food by capillary gas chromatography. Methods Samples were extracted with petroleum ether - acetone (1 + 1, V / V). The sample solution was sulfonated with sulfuric acid, purified by centrifugation or gel purification chromatography (GPC), and split / splitless. The medium polar capillary column (DB1701, BP-608), temperature-programmed chromatographic separation, electron capture detector detection, external standard quantification. Results The results showed that there was a good linearity between 0.005μg / ml and 0.10μg / ml for DDT, the correlation coefficient was> 0.999; the average recovery was 85.6% ~ 97.9%; RSD was 3.83% ~ 7.37% (n = 6 ); The detection limit of 666 was 0.003 mg / kg, and the total detection limit of DDT was 0.006 mg / kg. Conclusion The optimized method to solve the existing national standard detection methods deficiencies, simple operation, high resolution, good reproducibility, and can meet the daily health food residues in the detection of organochlorine pesticides.