WO1992022806A1 - Test pour peracides - Google Patents

Test pour peracides Download PDF

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Publication number
WO1992022806A1
WO1992022806A1 PCT/US1992/004891 US9204891W WO9222806A1 WO 1992022806 A1 WO1992022806 A1 WO 1992022806A1 US 9204891 W US9204891 W US 9204891W WO 9222806 A1 WO9222806 A1 WO 9222806A1
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WO
WIPO (PCT)
Prior art keywords
test
acid
per
per acid
recited
Prior art date
Application number
PCT/US1992/004891
Other languages
English (en)
Inventor
James Edward Christner
Leonard John Ii Lucchese
Original Assignee
Serim Research Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Serim Research Corporation filed Critical Serim Research Corporation
Publication of WO1992022806A1 publication Critical patent/WO1992022806A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3508—Organic compounds containing oxygen containing carboxyl groups

Definitions

  • the present invention involves test systems and devices for the rapid and facile threshold level testing of solutions of per acids in the presence of hydrogen peroxide. More specifically it relates to reagent strip test devices which are capable of giving a response which indicates that the solution being tested, which may also contain hydrogen peroxide, is or is not at a specified level or concentration of per acid.
  • Per acids are becoming increasingly important as cold sterilants in such diverse areas as health care and food processing. Because of their chemical nature and how these materials are produced, they are usually quite unstable and exist as combinations of per acid and hydrogen peroxide.
  • peracetic acid can be prepared by allowing acetic acid to react with 30 to 90 percent hydrogen peroxide solution in the presence of sulfuric acid. This reaction is, however, reversible and peroxy acids such as peracetic acid gradually hydrolyze to the corresponding carboxylic acid and hydrogen peroxide. For this reason, when such chemicals are used as sterilants, it is absolutely necessary to measure the amount of per acid present to ensure that the proper concentration or level of sterilant is present. This is especially true in the present health care environment which for cost containment reasons encourages reuse of otherwise disposable devices such as dialysis membranes.
  • test system One common type of test system or device presently in use in the health care area is the reagent strip.
  • the reagent composition which reacts specifically with the analyte of interest to give a colorimetric response is incorporated into a matrix such as paper and a small section of the dried paper is attached to a plastic strip for ease of handling.
  • the reagent strip is immersed momentarily into the solution of analyte and withdrawn.
  • the usual procedure is then to visually compare any color generated in the matrix to a standardized set of color blocks to determine the concentration of analyte in the solution being tested.
  • Such a procedure is quite useful when a wide range of analyte concentrations are encountered in the test samples and each level involves useful information for the analyst.
  • sterilant potency tests are commonly designed to give a so-called “go" or "no go” result. This enables the user to easily determine if the cold sterilant solution has the proper level or concentration of chemical present or if the solution must be either rejuvenated or discarded. Because of similarities in reactivity between per acids and peroxides, elaborate and cumbersome methods have been devised to assay or measure per acids in the presence of hydrogen peroxide.
  • Such methods usually rely on removal of the peroxide prior to determining the per acid or utilizing differences between per acid and peroxide in the speed of reaction of the test reagent therewith.
  • schemes are utilized which involve cooling the sample solution down to between 0 to 5 °C prior to adding the test reagents. This cooling step then allows the determination of per acid in the presence of peroxide.
  • the method involves adding excess potassium iodide to a sample solution of per acid and hydrogen peroxide cooled down to less than 5 °C.
  • the iodine liberated by the per acid is then titrated with 0.1 N sodium thiosulfate with starch as an indicator.
  • This portion of the procedure which involves the determination of per acid relies on the fact that per acids react much more rapidly than hydrogen peroxide at a temperature of less than 5 °C.
  • a second step is then used to determine the peroxide present in the test sample.
  • the paper also gives a background discussion relative to per acid analyses and cites relevant literature references.
  • the present invention relates to reagent strip test devices which are set to give a colorimetric response to a predetermined level of per acid in the presence of hydrogen peroxide.
  • the method of analysis is rapid and facile and does not involve temperature controls. More specifically, the reagent strip test devices described herein involve the following test composition incorporated into a matrix: a water soluble iodide in a quantity in excess of that required to react with the per acid present to generate iodine, a predetermined amount of a water soluble thiosulfate which reacts with the iodine generated and which amount depends on the level of peracid being detected and preferably an indicator which responds to any iodine in excess of that reacting with the thiosulfate.
  • the preferred reagent strip matrix is paper and the preferred indicator is soluble starch.
  • the analytes of the present invention are per acids which may be described by the following structure:
  • R is hydrogen, methyl, ethyl, phenyl, carboxyphenyl and furan.
  • per acids are: peroxyformic acid, peroxyacetic acid. peroxyphthalic acid, peroxybenzoic acid, peroxypropionic acid and peroxyfuroic acid.
  • water soluble components are usually preferred since impregnation into the supporting matrix is thereby facilitated.
  • any water soluble iodide can be employed with the preferable materials being potassium or sodium iodide.
  • the water soluble thiosulfate may be any of a variety of materials which when dissolved release the thiosulfate ion. Potassium thiosulfate is the preferred compound because of its availability and cost.
  • the excess iodine generated may be detected directly by its characteristic brown color, it is preferable to add an indicator to the test composition.
  • the indicators of the present invention are any of a variety of materials which respond to the presence of iodine in solution to give a colorimetric response, with the understanding that black is included as a color.
  • indicators are starch such as Thyodene (a partially hydrolyzed starch) and polyvinylpyrrolidone may be used with soluble starch the preferred material.
  • compositions described herein are incorporated into a matrix to give the reagent strip format.
  • the matrix is usually a flat, thin sheet-like material which is used to contain the test composition and allow the test solution containing the analyte to contact and react with the reagent system.
  • incorporation it is meant that the composition is either impregnated into a preformed matrix and dried or is mixed into a liquid polymeric material and cast as a film and dried to form the matrix.
  • the preformed matrix materials commonly used are paper or cellulosic materials, glass fibers and either woven or non-woven synthetic fibrous materials.
  • the polymeric matrices are made from a variety of polymers which when cast as a film are porous and allow the fluid being tested to penetrate the matrix and react with the test composition. When such a polymeric matrix is used, it is common practice to mix the test reagent composition with the liquid polymer prior to film formation.
  • the matrix may comprise attaching the test composition either chemically or physically to polymeric beads or granules and supporting the resultant materials on a support.
  • the matrix is preferably attached to a support usually consisting of a a plastic sheet material such as polystyrene which allows the user to immerse the matrix containing the test reagent composition into the test fluid for a predetermined period of time, withdrawing it and comparing the color formed to a standardized chart for comparison purposes.
  • a support usually consisting of a a plastic sheet material such as polystyrene which allows the user to immerse the matrix containing the test reagent composition into the test fluid for a predetermined period of time, withdrawing it and comparing the color formed to a standardized chart for comparison purposes.
  • the color chart may be omitted.
  • the concentration of the thiosulfate in the test reagent mix there is a wide latitude of ingredient concentrations which may be used to prepare the test reagent compositions of the present invention.
  • the iodide should be present in a range of concentrations of about from 2.2 grams per liter to 9.0 grams per liter and, if an indicatoris used, it should be present in an amount sufficient to give the desired visual response.
  • a buffer may also be advantageously used to keep the pH of the test composition in a range of about from 3 to 7. Representative of such buffers which may be used are citrate, acetate, phosphate, succinate and formate, with citrate a preferable buffer.
  • the thiosulfate concentration in the test composition is adjusted such that the iodine released from the reaction of the per acid with the iodide is consumed unless the concentration of the per acid is at a predetermined minimum level or concentration.
  • the excess iodine is either detected by its characteristic color or causes the indicator to respond indicating that the sterilant is present in a quantity sufficient to effect the desired sterilizing result. Accordingly, the thiosulfate concentration is adjusted to reflect the level of per acid being determined.
  • the concentration of thiosulfate with respect to per acid is set as follows: since one gram-molecular weight (mole) of per acid reacts with iodide to form one mole of iodine which in turn oxidizes two moles of thiosulfate, the thiosulfate must be present in a molar concentration twice that of the amount of per acid to be detected.
  • test composition of the present invention When the test composition of the present invention is contacted with a solution of per acid and peroxide, it has surprisingly been found that, at room temperature, the per acid reaction proceeds rapidly in comparison to the peroxide reaction so that there is no need to cool the test composition and test fluid to that required by the prior art, i. e. 0 to 5 °C. This is extremely advantageous since it allows the on-site testing of sterilant fluids and does not require a laboratory setting accompanied by the delays and costs associated therewith.
  • a sheet of Whatman #54 absorbant filter paper was saturated with a solution of the following ingredients: 5.0 grams sodium thiosulfate, 4.5 grams potassium iodide, 22.6 grams ammonium citrate, 250.0 ml 1% soluble starch solution and 750.0 ml distilled water.
  • the saturated paper was dried at 65 °C for 15 minutes and cut into one fifth inch squares.
  • the square reagent pads were then attached to the end of three by one-fifth inch strips of transparent sheet material which acted as handles for the test devices.
  • the reagent strip test pad areas were dipped into a solution of 800 ppm peracetic acid (PAA) at 20 °C, the pad immediately changed from white to a dark blue color.
  • PAA ppm peracetic acid

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Microbiology (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Biophysics (AREA)
  • Pathology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nutrition Science (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

Dispositif et système de test permettant de déterminer un niveau seuil de peracide dans une solution pouvant contenir du peroxyde. Plus précisément, on fait appel à un réactif en bande et à un mécanisme indicateur permettant de déterminer si le peracide se situe à un niveau ou à une concentration critique prédéterminé.
PCT/US1992/004891 1991-06-17 1992-06-09 Test pour peracides WO1992022806A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US71647191A 1991-06-17 1991-06-17
US716,471 1991-06-17

Publications (1)

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WO1992022806A1 true WO1992022806A1 (fr) 1992-12-23

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996027794A1 (fr) * 1995-03-04 1996-09-12 Merck Patent Gmbh Procede et equipement pour mettre en evidence la presence d'iodure
EP0916946A2 (fr) * 1997-11-12 1999-05-19 Integrated Biomedical Technology, Inc. Bande d'analyse pour le peroxyde d'hydrogène et le chlore
US6047436A (en) * 1997-11-11 2000-04-11 Alliedsignal Inc. Automotive windshield wiper blade with service life indicator
US6790411B1 (en) 1999-12-02 2004-09-14 3M Innovative Properties Company Hydrogen peroxide indicator and method
US7186373B2 (en) 2003-07-22 2007-03-06 Steris Inc. Visual detector for vaporized hydrogen peroxide
WO2009023503A1 (fr) * 2007-08-16 2009-02-19 American Sterilizer Company Indicateur pour surveiller un procédé de stérilisation
US7850925B2 (en) 2007-06-15 2010-12-14 American Sterilizer Company Apparatus for removal of vaporized hydrogen peroxide from a region
CN103048318A (zh) * 2012-12-20 2013-04-17 哈尔滨医科大学 井矿盐中碘含量快速定量检测方法
US10285401B2 (en) 2015-09-10 2019-05-14 Ecolab Usa Inc. Self indicating antimicrobial chemistry
US10866223B2 (en) 2016-12-15 2020-12-15 Ecolab Usa Inc. Colorimetric detection and quantitative estimation of peracids using a redox sensitive leuco dye
US11041837B2 (en) 2016-07-21 2021-06-22 Lonza, Llc Method and kit for determining peracetic acid concentration in disinfectant solutions

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU253426A1 (ru) * О. Д. Шапилов , Я. Л. Костюковский Способ количественного определения органических надкислот в присутствии перекиси водорода
US3121615A (en) * 1960-09-02 1964-02-18 Mine Safety Appliances Co Colorimetric moisture indicator
US3183173A (en) * 1963-06-10 1965-05-11 Miles Lab Test composition for detecting hydrogen peroxide
US3814668A (en) * 1969-10-15 1974-06-04 Miles Lab Method and device for the semi-quantitative determination of glucose in aqueous fluids
US4098575A (en) * 1975-06-19 1978-07-04 Zaidan-Hoijin Sugiyama Sangyo Kagaku Kenkyusho Peroxide value determining test for oils and fats
US4303753A (en) * 1980-03-20 1981-12-01 Miles Laboratories, Inc. Method and device for the semiquantitative determination of glucose in aqueous fluids
US4900682A (en) * 1987-12-19 1990-02-13 Merck Patent Gesellschaft Mit Beschrankter Haftung Method and reagent for the determination of peracids

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU253426A1 (ru) * О. Д. Шапилов , Я. Л. Костюковский Способ количественного определения органических надкислот в присутствии перекиси водорода
US3121615A (en) * 1960-09-02 1964-02-18 Mine Safety Appliances Co Colorimetric moisture indicator
US3183173A (en) * 1963-06-10 1965-05-11 Miles Lab Test composition for detecting hydrogen peroxide
US3814668A (en) * 1969-10-15 1974-06-04 Miles Lab Method and device for the semi-quantitative determination of glucose in aqueous fluids
US4098575A (en) * 1975-06-19 1978-07-04 Zaidan-Hoijin Sugiyama Sangyo Kagaku Kenkyusho Peroxide value determining test for oils and fats
US4303753A (en) * 1980-03-20 1981-12-01 Miles Laboratories, Inc. Method and device for the semiquantitative determination of glucose in aqueous fluids
US4900682A (en) * 1987-12-19 1990-02-13 Merck Patent Gesellschaft Mit Beschrankter Haftung Method and reagent for the determination of peracids

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
DANIEL SWERN, ED., "Organic Peroxides", published 1970, by WILEY-INTERSCIENCE: NEW YORK, pp. 369, 461, 464, 468, 497-516. *
FEIGL et al., "Spot Tests in Organic Analysis", published 1966, by ELSEVIER SCIENTIFIC PUBLISHING COMPANY: NEW YORK, page 615. *
SWOBODA et al., "Determination of the Peroxide Value of Edible Fats by Colorimetric Iodometric Procedures", published 1959, by CHEM. & INDUSTRY, pages 1090-91. *
TREADWELL, F.P., "Analytical Chemistry", Vol. 1, published 1930, by JOHN WILEY & SONS, INC.: New York, pp. 89-90. *

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996027794A1 (fr) * 1995-03-04 1996-09-12 Merck Patent Gmbh Procede et equipement pour mettre en evidence la presence d'iodure
US5939328A (en) * 1995-03-04 1999-08-17 Merck Patent Gesellschaft Mit Beschrankter Haftung Method for the determination of iodide
US6047436A (en) * 1997-11-11 2000-04-11 Alliedsignal Inc. Automotive windshield wiper blade with service life indicator
EP0916946A2 (fr) * 1997-11-12 1999-05-19 Integrated Biomedical Technology, Inc. Bande d'analyse pour le peroxyde d'hydrogène et le chlore
EP0916946A3 (fr) * 1997-11-12 2001-06-13 Integrated Biomedical Technology, Inc. Bande d'analyse pour le peroxyde d'hydrogène et le chlore
US6790411B1 (en) 1999-12-02 2004-09-14 3M Innovative Properties Company Hydrogen peroxide indicator and method
US7481975B2 (en) 1999-12-02 2009-01-27 3M Innovative Properties Company Hydrogen peroxide indicator and method
US7186373B2 (en) 2003-07-22 2007-03-06 Steris Inc. Visual detector for vaporized hydrogen peroxide
US7988911B2 (en) 2007-06-15 2011-08-02 American Sterilizer Company Method for removal of vaporized hydrogen peroxide from a region
US7850925B2 (en) 2007-06-15 2010-12-14 American Sterilizer Company Apparatus for removal of vaporized hydrogen peroxide from a region
US7988920B2 (en) 2007-06-15 2011-08-02 American Sterilizer Company Device for aerating a region after injection with vaporized hydrogen peroxide
WO2009023503A1 (fr) * 2007-08-16 2009-02-19 American Sterilizer Company Indicateur pour surveiller un procédé de stérilisation
US8512633B2 (en) 2007-08-16 2013-08-20 American Sterilizer Company Indicator for monitoring a sterilization process
CN103048318A (zh) * 2012-12-20 2013-04-17 哈尔滨医科大学 井矿盐中碘含量快速定量检测方法
CN103048318B (zh) * 2012-12-20 2015-08-26 哈尔滨医科大学 井矿盐中碘含量快速定量检测方法
US10285401B2 (en) 2015-09-10 2019-05-14 Ecolab Usa Inc. Self indicating antimicrobial chemistry
US10555523B2 (en) 2015-09-10 2020-02-11 Ecolab Usa Inc. Self indicating antimicrobial chemistry
US11576378B2 (en) 2015-09-10 2023-02-14 Ecolab Usa Inc. Self indicating antimicrobial chemistry
US11041837B2 (en) 2016-07-21 2021-06-22 Lonza, Llc Method and kit for determining peracetic acid concentration in disinfectant solutions
US10866223B2 (en) 2016-12-15 2020-12-15 Ecolab Usa Inc. Colorimetric detection and quantitative estimation of peracids using a redox sensitive leuco dye
US11674935B2 (en) 2016-12-15 2023-06-13 Ecolab Usa Inc. Colorimetric detection and quantitative estimation of peracids using a redox sensitive leuco dye

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