(12) United States Patent (10) Patent No.: US 6,420,181 B1 Novak (45) Date of Patent: *Jul
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USOO642O181B1 (12) United States Patent (10) Patent No.: US 6,420,181 B1 Novak (45) Date of Patent: *Jul. 16, 2002 (54) FIELD MICROSPOT TEST METHOD FOR (56) References Cited ON-SITE CHEMICAL TESTING U.S. PATENT DOCUMENTS (75) Inventor: Thaddeus John Novak, Bel Air, MD (US) 4,346,001 A * 8/1982 Tyihak et al. ............... 210/658 4,428,908 A * 1/1984 Ashley et al. ................ 422/61 (73) Assignee: The United States of America as represented by the Secretary of the Army, Washington, DC (US) sk cited- by examiner (*) Notice: Subject to any disclaimer, the term of this Primary Examiner-Lyle A. Alexander patent is extended or adjusted under 35 XX U.S.C. 154(b) by 0 days (74) Attorney, Agent, or Firm Ulysses John Biffoni; a -- William W. Randolph Rpatent is Subject to a terminal dis- (57) ABSTRACT A method, System and kit for detecting the presence of an (21) Appl. No.: 09/296,602 analyte includes placing a Solution containing the analyte in 1-1. a microcapillary tube and placing the microcapillary tube in (22) Filed: Apr. 23, 1999 contact with a layer of Sorbent material So that the Solution Related U.S. Application Data is withdrawn from the microcapillary tube by capillary action. The Sorbent material and Solvent for the Solution are (63) Continuation-in-part of application No. 08/763,181, filed on Selected so that the Solvent is absorbed into the Sorbent Dec. 11, 1996, now Pat. No. 5,935,862. material and the analyte is adsorbed by the Sorbent material (51) Int. Cl." ......................... G01N33/00, G01N 30/90 and concentrated at the Spot where the microcapillary tube (52) U.S. Cl. ....................... 436/104; 436/162; 436/164: contacts the Sorbent material. A detector reagent is applied 436/66. 436/165. 210,658 to the Sorbent material to indicate the presence of the (58) Field of Search ................................. 210/656, 658, analyte. 210/634, 635; 422/56, 58, 61, 68.1, 70; 436/103-105,161-164, 166, 169, 808 16 Claims, 2 Drawing Sheets U.S. Patent Jul. 16, 2002 Sheet 1 of 2 US 6,420,181 B1 A/G. f. 27 U.S. Patent Jul. 16, 2002 Sheet 2 of 2 US 6,420,181 B1 A/G. 4 NEGATIVE TEST POST VETEST US 6,420,181 B1 1 2 FIELD MICROSPOT TEST METHOD FOR having a Surface layer formed of a Sorbent material or gel. ON-SITE CHEMICAL TESTING In order to Separate the components of the analyte obtained from a Sample, a drop of Solution is carefully applied above This is a Continuation-In-Part of U.S. application Ser. the bottom edge of a thin layer chromatography plate. No. 08/763,181, filed Dec. 11, 1996 now U.S. Pat. No. 5 Solutions Suspected of containing target analytes are pref 5,935,862. erably deposited onto the surface of a TLC plate in the form of a drop to avoid a streaking pattern that would result if the GOVERNMENT INTEREST device for applying the drop actually contacts the Surface of the plate while a Sample Solution is being deposited. After The invention described herein may be manufactured, the Solvent evaporates, the residue on the plate is eluted with licensed, and used by or for the U.S. Government. another Solvent or Solvent mixture (also known as the eluant) thereby causing the chemical components of the BACKGROUND OF THE INVENTION Sample to migrate towards the top or opposite edge of the 1. Field of the Invention plate. When the proper conditions and eluant are chosen, This invention relates to a field test kit and method of 15 each analyte migrates across the plate at a rate that is on-site testing for the presence of contaminants and different from the other analytes. The elution step results in chemicals, and more particularly to a micro spot method for the different analytes Separating from each other and Settling detecting the presence of a variety of chemicals and envi at different regions and as diffuse spots along the path of ronmental contaminants. migration. After the elution Step, the plates are allowed to dry and then they are Sprayed with a Solution of visualization 2. Description of the Prior Art reagent (detector reagent). A persistent concern with thin In View of biological hazards associated with toxic chemi layer chromatography is that the elution Step of waiting for cals and environmental contaminants, regulations have been the Solvent to completely wet the plate and for the analytes established by legislatures and environmental agencies to to migrate and Separate is relatively time-consuming. In monitor a wide variety of chemicals and their byproducts. AS 25 many instances, proper completion of the elution phase may a result, it is often necessary to conduct on-site inspections exceed an hour and warrant involved techniques and quality and analyses of various chemical Spills, dump Sites, and control Steps to assure adequate Separation of the different manufacturing facilities to detect environmental analytes. Another concern involves situations where the contaminants, hazardous conditions and to assure compli analytes are present in Such low concentrations that the ance with environmental regulations. detection Signals obtained in the tests are weak and can Advantages of on-site inspection and analysis of chemical possibly be misread. In Summary, with thin layer chroma Sites include resolving ambiguities during the inspection, tography the analytes in the Sample migrate and Separate reducing the potential for contamination and croSS into localized regions, as opposed to concentrated at Spots or contamination of Samples during travel to off-site testing points. laboratories, and providing a convenient method of perform 35 ing a large number of preliminary tests to detect and Screen SUMMARY OF THE INVENTION for chemical contaminants. On-site inspection also provides The micro Spot test System and methodology of the a rapid indication of those Samples which may possibly present invention relates to an apparatus and method for the contain compounds that must be identified using more on-site testing of analytes contained in a Sample by dissolv Sophisticated laboratory analytical techniques. On-site test 40 ing the analytes in a Solvent and utilizing capillary deposi ing also allows the level of concentration and Spread of tion techniques to concentrate the analytes on Sorbent mate contamination from chemical Spills to be readily Surmised. rials. Detection Sensitivity and accuracy for a range of Reagent-based chemical detection and chromatographic concentrations of analytes is provided by applying a Solution methodologies are attractive for on-site testing and Screen containing the analytes to a Sorbent layer by capillary ing because many tests can be run in a short period of time 45 deposition So that the analytes in the Solution become and they are capable of providing Visual presumptive evi concentrated at the particular spot or point of deposition on dence of the presence of a chemical Substance in a Sample. the Sorbent layer. The Solutions are deposited by placing One methodology comprises classical Spot tests that are Small diameter tubes containing the analyte Solution in normally carried out in depressions or wells of a porcelain contact with the Surface of the Sorbent material So that the Spot plate. Conventionally, Small amounts of a Solution, 50 solutions are drawn from the small diameter tubes by which may contain chemical contaminants, are placed in the capillary action. A detector reagent is then utilized to detect Wells of the Spot plate. Small quantities of different reagents the presence of the analytes that are concentrated at the Spot are then added to the Solution Samples and a positive test is where the Small diameter tube contacts the Sorbent layer. normally signified by a color change in the well of the Spot A System for chromogenically detecting the presence of plate. An advantage with these tests is that a number of tests 55 chemical analytes includes a means for obtaining a Sample can be carried out on a single plate. For example, as many Solution containing the analytes, a device for the capillary as 12 different Spot tests can be carried out on a Small deposition of the Sample Solution, chromatographic Sorbent 3.5x4.5 inch spot plate. Another advantage is that it is materials, and chromogenic detector reagents. Storage possible to rapidly Screen a large number of Samples during devices may be provided for the Samples and for Sample a short period of time. However, as the concentration of the 60 Solutions, capillary deposition devices, the chromatographic chemical Substances become more dilute, it becomes more Sorbent materials and the chromogenic detector reagents. difficult to reliably detect the presence of the chemical Accordingly, one object of the present invention is to Substances. In most cases, the lower limit of detection is in provide a compact chemical Screening apparatus which is of the 1-100 microgram range. a Self-contained, efficient design for rapid Screening of Another methodology for Screening Samples and detect 65 Solutions for the presence or absence of target analytes. ing target analytes in Samples is use of thin layer chroma Another object of the present invention is to provide a tography (or TLC), which conventionally utilizes a plate chemical Screening device which is relatively simple to use US 6,420,181 B1 3 4 for Sample Solutions containing a wide range of analytes in Washing, extracting, or eluting a Sample with a Solvent or a wide range of concentration levels. mixture of solvents. For example, surface wipes 18 or Swabs These, together with still other objects of the invention, 19 of polyester or similar material are used to obtain a along with the various features which characterize the Sample by wiping a Suspected Surface.