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Pesticide Residues in Food: Technologies for Detection (Part 7

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Pesticide Residues in Food: Technologies for Detection (Part 7 Chapter 5 Automation in Today’s Pesticide Laboratory CONTENTS Pago Individual Component Automation . , ... , 49 The Role of Automation . 49 Multiple Component Automation—Robotics . 51 Robotics in the Pesticide Residue Laboratory . 51 Two Principles for Successful Use of Robotics . 54 Benefits and Limitations of Robotics in the Analytical Laboratory . 54 Chapter 5 References . ..,.0.. .,,*.,,, ● ....*.. ● .*..**, ..,**,, 55 Boxes Box ~ Page 5-A. The Ideal, Fully Automated Analytical Laboratory . 49 5-B. Zymate’s PyTechnology Robotics System . 52 -.. -“ . Figure Figure Page 5-1. Schematic Drawing of Zymate Robotic System. .,,..,. ● ....*. 53 Tables Page 5-1, Laboratory Unit Operations (LUOs) of Robotic Systems ..*,.*. 51 5-2, Comparison of Robot and ..,*., ,.,.... 53 Chapter Automation in Today% Pesticide Laboratory INDIVIDUAL COMPONENT AUTOMATION Automation has greatly increased analytical productivity of pesticide residue laboratories, Box 5-A.—The Ideal, Fully Automated and most such laboratories today use some type Analytical Laboratory of automated equipment. Computers, for in- A fully automated laboratory, now existing stance, have made the identification and quan- only on paper, is one that would automatically tification of pesticides easier. Automated geI process a sample from its entrance into the permeation chromatography and autoinjection laboratory through the production of a writ- of samples onto chromatography have allowed ten final report. An automated process of this type would move the sample through a series unattended work to take place day and night of operations whereby it could be subsampled, and permitted analysts to do additional work. chopped, ground, blended, filtered, centrifuged, and extracted. The extract then could be evap- The Role of Auomation orated, partitioned, redissolved, diluted, dried, chemically treated, subsampled and chroma- Despite such advances in automation, the tographed, Data from the chromatography would prospect of designing a fully automated ana- go to a computer, which would identify the lytical laboratory remains an ideal (box 5-A). sample, perform calculations on its abundance, The procedures for analyzing a food sample graph the results, collate it with other data, are time-consuming, and many steps must still and produce a hardcopy. Leftover sample or be done manually. A major percentage of the sample extracts would automatically be moved total analysis time is spent in preparation, ex- back to a refrigerator, freezer or other proper traction, and cleanup. Food is generally sub- storage area, where it would be available for reanalysis if the computer data did not meet cer- sampled, cut into manageable pieces if neces- tain quality assurance/quality control standards. sary, and subsequently blended with solvent to extract the pesticide. The sample is then filtered Only very few regulatory laboratories have or centrifuged, and the extract is either parti- experience with robotic automation systems. tioned with another solvent or concentrated by Given the current cost and capability of auto- evaporation. An optional cleanup step to iso- mation instrumentation and technology, it is late the pesticide may be required. Finally, the not yet possible to automate regulatory labora- tories totally. sample is injected into a gas or liquid chromato- graphy for analysis. Automating the sample preparation and ex- traction steps would generate the greatest time chromatography (GPC) can be automated (16) savings, but these steps are the most difficult (for a description of gel permeation chromatog- to automate because many types of samples re- raphy see ch. 3); in fact, FDA and FSIS use auto- quire different preparation (10). Consequently, mated GPC, primarily for fatty foods. Require- improvements in automation have focused pri- ments for quick results may pose a problem, marily on the cleanup and determination stages however, because automated GPC processes of pesticide residues in food analysis. only one sample at a time. Several types of automated equipment can Further automation of the cleanup step may be used in the cleanup step. Gel permeation be possible with the recent development of an 49 50 evaporation device that can be connected to ing as many as 100 miniature vials and capped the automated GPC. This evaporation device to seal-in volatile organic solvents and pesti- replaces the gel permeation solvent with one cides. These trays can be refrigerated to pre- more suitable for gas chromatography, concen- vent the decomposition of thermally unstable trates the sample through evaporation, and de- pesticides. Automated sample injectors, also posits each sample into a sealed vial, which then known as autosamplers, can then inject the can be injected into a chromatography for anal- sample into an automated chromatography for ysis. Such a device can process various types unattended analysis. Autosamplers have the of pesticides with excellent reproducibility and added advantage of being more precise in their recoveries (3). At present, FDA has not used volumetric sampling than a chemist, resulting automated evaporation equipment, in part be- in higher quality analytical data. Autosamplers, cause it does not want to use its capital budget however, do not appear to be used for the to replace still functional manual evaporators majority of food samples at regulatory labora- and concentrators. FSIS laboratories do, how- tories. In some cases, they are considered ever, use such equipment. slower and more expensive than hand injec- tion (9). Another automated device for cleaning up food extracts is the DuPont Autoprep System. Automation of the detection step has been This device, used by some FSIS labs, uses cen- greatly facilitated by computerized data proc- trifugal force rather than gas pressure or essing. Gas and liquid chromatography are vacuum, as is done by other devices designed equipped with computers known as integrators. for this purpose. As many as 12 samples can Integrators determine the retention time of an be processed at a time, only small volumes for unknown chemical, necessary for its identifi- each wash are required (1 to 5 milliliters), and cation, and the quantity of the chemical. The the pesticide is effectively concentrated for integrator can then provide this information analysis by chromatography or other means. in report form. An integrator can be programmed to identify any specified retention time, allow- The detection step has also been automated. ing easier analysis of a specific pesticide. Mass Samples to be analyzed using gas or liquid chro- spectrometer and infrared detectors are equipped matography can be loaded on sample trays hold- with computers for sample identification that can search a library to match a sample to a known mass spectra. Data processing’s impor- tance is seen as increasing with the develop- ment of the laboratory information manage- ment system (LIMS). The LIMS goes beyond recording data; it produces tables that could be included in reports, it tracks samples, and it provides an electronic “paper trail” for ful- filling the requirements of “good laboratory practices.’” In addition, a properly designed LIMS can be linked with virtually any type of analytical instrument from any manufacturer and can be used to collect and interpret data from it. Pesticide residue laboratories have not Photo credit: Analytica/ Blo-Chemistry Laboratories, Inc. ‘These are standards describing the quality of instrumental, ABC Laboratories’ GPC/Autovap@ system combines procedural, analytical, and personnel performance prescribed a gel permeation chromatography module with an for laboratories conducting studies that support or are intended evaporation module to allow automated sample to support applications for research or marketing permits for cleanup and concentration for a maximum of (a) pesticide products regulated by the EPA (4o C.F.R. Section 23 sample extracts. 160) and (b) products regulated by the FDA (21 C.F.R. Section 58). 51 yet adopted LIMS because of its early stage of mated ones on a small scale, although automa- application and its high cost (4). tion may provide other benefits, e.g., reducing analyst exposure to hazardous solvents. There- Further improvements in analytical methods fore, decisions to increase the use of automated are possible through automation, but some con- equipment must consider the goals of monitor- straints exist. Given that much of the automated ing programs and the moneys available. For ex- equipment including robots has high capital ample, if increased sample throughput were the costs, Federal regulatory laboratories with low primary goal of a monitoring program, then fur- or fluctuating capital budgets may have diffi- ther advances in automation maybe necessar culty purchasing such equipment. Second, y before its adoption. manual procedures may be faster than auto- MULTIPLE COMPONENT AUTOMATION-ROBOTICS Robotics is a special type of automation that cal procedure. Table 5-1 explains most of the allows mechanical manipulation of an object LUOs that robotic systems can now perform. in a multitask computer-assisted, and repro- The most popular laboratory robotics system grammable manner (6). In the laboratory, the is produced by the Zymark Corporation and is robot uses systems technology to allow multi- a modular system that combines robotics, pro- ple devices to perform such simple laboratory grammable computers, and peripheral instru- operations as weighing, dissolving, diluting, ex- ments to carry out laboratory procedures
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