Solid-phase Extraction-hplc Analysis Of Pesticide Residues In The Research And Application

Presently, the pesticide residue is an interested topic, which is given muchattention in food security in all the world. Because it is closely related with humanhealth and international agricultural products trade. In these years, to protect theconsumers' health, Chinese government has been strengthening more and more in theadministration and guidance of the pesticide residues. What is more, thecompetitiveness of our agricultural products is promoting in the global market throughemilination of technical barrier in the agricultural products export. The standards ofpesticide residues detection and the pesticide residues limitation are necessary for theregulation of the pesticide residues in agricultural produce. Thus, at present, itbecomes especially important to study the pesticide residues problem arouses inChinese agricultural produce, the detection techniques required by the internationalagricultural produce trade as well as the degradation dynamics and the residuelimitation of the pesticide residue in the environment.Pesticide residue assay is an analysis technique that determines the tracecomponents in complex mixture, which requires high sensitivity, efficient recovery,good reappearance as well as a simple and workable operation. To achieve these aims,the choices of pretreatment techniques and detection techniques are critical. The studyon pesticide residue detection methods and the study on the degradation dynamics andthe residue limitation of pesticide in the environment play important roles in directingthe peasants to use the pesticides in a scientific and rational way,enhancing thequality of Chinese agricultural produce and its competitiveness in the global marketand promoting international agricultural international trade.The dissertation includes two parts: the background and literature summarize(ChapterⅠtoⅢ) , and three methods of determination for pesticide residues (ChapterⅣ toⅥ ).The main subjects of study:I This part is a brief introduction of the fundamental conceptions, the mainresources, the current situations and the major hazards of pesticide residue.II This part is an overview of the advances in the field of the sample pretreatmenttechniques and the detection techniques for the pesticide residue analysis.III This part is on the application of SPE and HPLC technique in the pesticideresidue analysis, which is an overview focusing on SPE technique and HPLCdetection technique.IV This part is on the determination of Famoxadone and its residue in the appleand soil by SPE-HPLC. A method is established, which determines the residueamount of Famoxadone, the effective ingredient of Equation contact, in apples andsoils by HPLC. With C18 SPE column as the purification condition, the detectiontechnique adopted is HPLC with the phenyl column as chromatographic column. Therecovery of this method is over 82%, while the relative standard deviation less than5.6% and the limit of detection is 0.02mg/kg. By this method, the final residueamount and analyzed the residue dynamic of Famoxadone in apples and soils weredetermined, which offers reference data to the safe and rational handling and theregulation of this pesticide.V This part is on the determination of Indoxacard and its residue in the vegetableby SPE-HPLC. A method is established, which determines the residue amount ofIndoxacard in spinach by HPLC. With OASIS column as the purification conditionand by optimizing the leaching conditions in both base and acid mediums, theinterfering substances are eliminated within a wider range and the selectivity andsensitivity are improved. The detection technique adopted is HPLC with the ODScolumn as chromatographic column. The recovery of this method is over 83%,while the relative standard deviation less than 7.7% and the limit of detection is0.01mg/kg. By this method, the final residue amount and analyzed the residuedynamic of Indoxacard in spinach were determined, which offers reference data to thesafe and rational handling and the regulation of this pesticide.VI This part is on the determination of Chlorfluazuron and its residue in thevegetable and fruit by SPE-HPLC. A method is established, which determines theresidue amount of Chlorfluazuron in Chinese date and cabbage by HPLC. WithOASIS column as the purification condition and by optimizing the leachingconditions in both base and acid mediums, the interfering substances are eliminatedwithin a wider range and the selectivity and sensitivity are improved. The detectiontechnique adopted is HPLC with the ODS column as chromatographic column. Therecovery of this method is over 85%, while the relative standard deviation less than9.8% and the of detection is 0.02mg/kg. By this method, the final residue amount andanalyzed the residue dynamic of Chlorfluazuron in Chinese date and cabbage weredetermined, which offers reference data to the safe and rational handling and theregulation of this pesticide.The research findings in this dissertation offer reference data to the setting of thepesticide residue limitation for vegetables and fruits. It also provides the supervisionsector with the reference data in terms of the scientific and standardized regulation ofthe pesticide residue in agricultural produce and the production management of thegreen food and pollution-free agricultural produce from the sources. What should bepointed out is that the application of SPE-HPLC technique in the pesticide residueanalysis, like the multi-residues determination technique for the properties of thepesticide adopted, still needs a further investigation.