Chromatography Detection And Toxicity Analysis Of Pesticide Residue In Vegetable Of Jimei District

In view of the phenomenon of various vegetable existing different of pesticide residues problem, the status and risk of 52 kinds of pesticide residue in six kind of vegetables in the production bases of Jimei District were monitored and evaluated; and a method for trace level, simultaneous and multiresidue analysis of 11 species underground pest pesticides in sweet potato(roots class vegetable) by Qu ECh ERS and HPLC-MS/MS(ultrahigh-performance liquid chromatography tandem mass spectrometry) were established; the toxicity study of sodium 4-chlorophenoxyacetate(4-CPANa), one of the poison bean sprouts(bud dish class vegetable) abuse of plant growth regulator, were finished.First of all, the pesticide residues in vegetables in the production bases of Jimei District, Xiamen City from 2012 to 2014 were analyzed. The index of food safety model and the risk index model were both applied to estimate the detection of pesticide. The result showed that the status of vegetable pesticide residue in the production bases of Jimei District from 2012 to 2014 was vulnerable to seasonal influences. The detectable rate of pesticide residue in the different type of vegetables from higher to lower was eggplant vegetables, leaf vegetables, melon vegetables, bean vegetables, tuber vegetables and other vegetables. 22 of 52 monitored pesticides were detected from the vegetable samples, and 3 were excessive. Results indicated that every kind of pesticides to the overall damage on the health of consumers was low risk within the past three years and the status of pesticide residue in vegetables of the production bases of Jimei District has presented a good condition.Then, a method for trace level, simultaneous and multiresidue analysis of 11 kinds of underground pesticides in sweet potato by Qu ECh ERS and HPLC-MS/MS were established; the sample pretreatment conditions and HPLC-MS/MS conditions were optimized. Sweet potato were extracted with acetonitrile directly, and purified by primary secondary amine with Qu ECh ERS method, Acetonitrile-water(0.1% HAc) was chose to be mobile phase with gradient elution, and then analyzed by using HPLC-MS/MS in multiple reaction monitoring mode via positive electrospray ionization(ESI+) with an Venusil MP C18 column(3 μm, 2.1 mm×100 mm) as the analytical column, and the quantization was carried out by the external standard method with the blank matrix. The chromatographic peaks of 11 kinds of underground pesticides were flowed out within 10 minutes. For the above method, the linear correlation coefficients for 11 kinds of pesticides were not less than 0.9990 in their linear scope with good linearity. Respectively, the limit of detection ranged from 0.007 μg/kg to 4.000 μg/kg. The limit of quantitation was in the range of 0.023~13.333 μg/kg. The recoveries of 11 kinds of underground pesticides in sweet potato matrices at four spiked levels of 5, 10, 20, 50 μg/kg ranged from 84.2% to 117.2%, and the relative standard deviations were in the range of 1.4%~8.3%. The results showed that the method is simple, rapid, and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis. This method was applicable to simultaneous confirm the residues of underground pesticides in sweet potato.Finally, acute, accumulative and subacute toxicity of 4-CPANa in mice and its residue in their body were investigated with Kun Ming mice as animal model. The oral acute toxicity of 4-CPANa in mice was determined by the modified Korbor method, and the oral accumulative toxicity in mice was carried out by an incremental exposure method with an initial dose of 107.4 mg/kg. Group low-dose, medial-dose, high-dose were gavaged with 4-CPANa solution 13.4, 71.6, 214.8 mg/kg respectively daily administration for 28 days on subacute toxicity test. The results showed that the half-lethal dose of 4-CPANa to mice was 1074.1 mg/kg and the accumulative coefficient K was larger than 8. The lowest observed adverse effect level of 4-CPANa was considered to be 71.6 mg/kg bw and no observed adverse effect level to be 13.4 mg/kg bw. Compared with the control group, 4-CPANa showed the different influences on physiological index and serum biochemical index of mice. Furthermore, 4-CPANa also can result in visible lesions and significant histopathological changes in the liver and kidney of mice. The 4-CPANa residue in mice was observed as follows in decreasing order: urine liquid>kidney>liver>blood>heart>brain>muscle. The results showed that 4-CPANa was classified to the 4th toxicity and belonged to the low accumulation compound, the toxic effect of 4-CPANa toward mice was mainly exhibited as lesions on liver and kidney.In conclusion, this thesis conducted monitoring, risk assessment, detection and toxicity reasearch according to the status of different pesticide residues in different kinds of vegetables, and provided a guarantee for safety production of all kinds of vegetables.