Abstract

The overall theme of this project was to increase the speed of analysis for monitoring pesticide residues in food. Traditionally, analytical methods for multiple pesticides are time-consuming, expensive, laborious, wasteful, and ineffective to meet critical needs related to food safety. Faster and better methods were needed to provide more cost-effective detection of chemical contaminants, and thus provide a variety of benefits to agriculture. This overarching goal to speed and improve pesticide analysis was successfully accomplished even beyond what was originally proposed by the investigators in 1998. At that time, the main objectives of this project were: 1) to further develop a direct sample introduction (DSI) device that enables fast sampling and introduction of blended-only agricultural products for analysis by gas chromatography (GC); 2) to evaluate, establish, and further develop the method of simultaneous pulsed flame photometric detector (PFPD) and mass spectrometry (MS) detection for enhanced pesticide identification capabilities; and 3) to develop a new and novel MS pesticide analysis method, based on the use of supersonic molecular beams (SMB) for sampling and ionization. The first and third objectives were successfully accomplished as proposed, and the feasibility of the second objective was already demonstrated. The capabilities of the GC/SMB-MS approach alone were so useful for pesticide analysis that the simultaneous use of a PFPD was considered superfluous. Instead, the PFPD was investigated in combination with an electron-capture detector for low-cost, simultaneous analysis of organophosphorus and organochlorine pesticides in fatty foods. Three important, novel research projects not originally described in the proposal were also accomplished: 1) development of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticides in foods; 2) development and optimization of a method using low-pressure (LP) GC/MS to speed pesticide residue analysis; and 3) innovative application of analyte protectants to improve the GC analysis of important problematic pesticides. All of the accomplishments from this project are expected to have strong impact to the analytical community and implications to agriculture and food safety. For one, an automated DSI approach has become commercially available in combination with GC/MS for the analysis of pesticide residues. Meanwhile, the PFPD has become the selective detector of choice for the analysis of organophosphorus pesticides. Great strides were made in SMB-MS through the manufacture of a prototype "Supersonic GC/MS" instrument, which displayed many advantages over commercial GC/MS instruments. Most notably, the QuEChERS method is already being disseminated to routine monitoring labs and has shown great promise to improve pesticide analytical capabilities and increase lab productivity. The implications of these developments to agriculture will be to increase the percentage of food monitored and the scope of residues detected in the food, which will serve to improve food safety. Developed and developing countries alike will be able to use these methods to lower costs and improve results, thus imported/exported food products will have better quality without affecting price or availability. This will help increase trade between nations and mitigate certain disputes over residue levels in imported foods. The improved enforcement of permissible residue levels provided by these methods will have the effect to promote good agricultural practices among previously obstinate farmers who felt no repercussions from illegal or harmful practices. Furthermore, the methods developed can be used in the field to analyze samples quickly and effectively, or to screen for high levels of dangerous chemicals that may intentionally or accidentally appear in the food supply.

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