Detecting Techniques Research Of Triazole Fungicide And Organochlorine Pesticides Residues In The Qian Food

In food analyses, sample preparation and pretreatment are crucial steps, the efficiency of which is directly infect the reliability,accuracy and throughput of analytical method. In the dissertation, the new triazole fungicide pesticides(myclobutanil and diniconazole) and the organochlorine pesticide(OCPs)(α-HCH、β-HCH、γ-HCH、δ-HCH、PP′-DDE 、 OP′-DDT 、 PP′-DDD 、 PP′-DDT 、 hexachlorobenzene 、heptachlor、quintozene、Trans-chlordane) which have been used for a long time and have a higher residual were selected as the research object. The solid extraction column packed with florisil and sulfuric acid were selected as the samples purification, and the samples were tested through the gas chromatograph electron capture dector(GC-ECD). The results were as follows:(1) The sorghum samples were extracted with acetonitrile and acetone, purified by a solid phase extraction column packed with florisil and detected by gas chromatograph electron capture dector through the capillary column. It turned out that the detection limit of myclobutanil(3S/N) was 0.002μg·g-1, and the spiked recoveries of sorghum samples were between 83.2% and 108.6% with relative standard deviation of 8.8%(n=6). Meanwhile, the detection limit of diniconazole was 0.00083μg·g-1, and average recoveries were in the range from 94.1% to 118.0% with relative standard deviation of 8.3%(n=6). The established methods were applied in other food products(corn,rice,wheat,buckwheat) testing and the results are as follows: the average recoveries of the diniconazole and myclobutanil were in the range from 70.2~103.8% and 78.0~96.5%.(2) The organochlorine pesticides in the sorghum samples were extracted by n-Hexane and acetone, purified by the sulfuric acid and tested by the GC-ECD. Results showed that the limitations were 0.091~0.621ng·kg-1, the average recoveries were 80.6~112.9% with the RSD(%) were 4.5~8.7%(n=9). This method was used in other grain(rice, wheat, corn, buckwheat) and the results as follows: recoveries of 11 kinds of organochlorine were 76.0~116.3%.(3)The method on detecting eleven organochlorine pesticide residues in houttuynia cordata was established. The samples were extracted with petroleum ether and acetone, purified by sulfuric acid and analysed with ECD. The results showed that the organochlorine pesticide residues detection limits in the range of 0.023μg·kg-1 to 0.286μg·kg-1, and the correlation coefficients were 0.9970~0.9998, and the average recoveries of the samples were 73.2~115.0% with RSD(%) were 1.4~14.2%(n=5).