NZ532151A - A method of quantitation of chemical preservatives within wood using enzyme linked immunosorbent assay technology combined with chromatographic analysis - Google Patents

A method of quantitation of chemical preservatives within wood using enzyme linked immunosorbent assay technology combined with chromatographic analysis

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Publication number
NZ532151A
NZ532151A NZ53215104A NZ53215104A NZ532151A NZ 532151 A NZ532151 A NZ 532151A NZ 53215104 A NZ53215104 A NZ 53215104A NZ 53215104 A NZ53215104 A NZ 53215104A NZ 532151 A NZ532151 A NZ 532151A
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NZ
New Zealand
Prior art keywords
wood
solvent
extraction
preservative
filtration
Prior art date
Application number
NZ53215104A
Inventor
Peter James Hayward
Jarrett Malcolm Black
Original Assignee
George William Mason John Brod
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Publication date
Application filed by George William Mason John Brod filed Critical George William Mason John Brod
Priority to NZ53215104A priority Critical patent/NZ532151A/en
Priority to AU2005201412A priority patent/AU2005201412B2/en
Publication of NZ532151A publication Critical patent/NZ532151A/en

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  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

A method of quantitation of chemical preservatives within wood, wood-based products and engineered wood products is disclosed, wherein the method comprises the use of chromatographic extraction methods combined with an enzyme linked immunosorbent assay comprising the steps of: (a) particle size reduction of the wood-based material; (b) soaking of the wood particles in a solvent; (c) separation of the solvent from the wood particles and filtration of the solvent; (d) dilution of the solvent into an aqueous medium; and (e) analysis of the chemical preservative by enzyme linked immunosorbent assay.

Description

New Zealand Paient Spedficaiion for Paient Number 532151 $2>&!§/ No: 532151 Date: 6 April 2004 NEW ZEALAND Patents Act 1953 COMPLETE SPECIFICATION METHOD FOR DETERMINING BIOCIDES WITHIN WOOD We, GEORGE WILLIAM MASON, JOHN BRODIE MATTHEWS, JOHN SUTHERLAND AULD, PETER JAMES HAYWARD AND CHRISTINE ANNE HAYWARD trading in partnership as TAPUAE PARTNERSHIP all New Zealand citizens of 78 Plymouth Road, R D 4, New Plymouth, New Zealand do hereby declare the invention, for which l/we pray that a Patent may be granted to me/us, and the method by which it is to be performed to be particularly described in and by the following statement:- Spec465(comp - revised) INTELLECTUAL PROPERTY OFFICE OF N.Z - 5 APR 2005 RECEIVED 31 March 2005 Title of the Invention Method of Determining Biocides Within Wood Background to the Invention The invention relates to a method for determining biocides within wood.
Presently, chemical preservatives are added to wood, wood-based products and engineered wood products to protect them. The preservatives can include insecticides, fungicides, mouldicides and bacteriocides.
For example, the preservatives can be insecticides to protect the products from attack by insect species. In order to ensure that such wood-based materials are treated with sufficient insecticide to inhibit attack, it must be possible to quantify the amount of insecticide that is infused into the material.
As is known in the art, the families of insecticide presently used are neonicotinoids, synthetic pyrethroids, organophosphates and phenyl pyrazoles. As the potency of the compounds within these families has increased, the quantity of the compounds required for protection of timber related materials has decreased remarkably. The resultant low dosages have made it difficult to detect the active ingredients in the timber related materials, let alone quantify them.
Spec465(comp - revised) 2 31 March 2005 Conventional methods of analysis for determination of the active content of wood-based materials rely on chromatography, specifically gas chromatography (GC) and high performance liquid chromatography (HPLC). Although such chromatographic techniques yield excellent results for the analysis of the above mentioned insecticides in water or sap extractions from vegetable based materials, they give reduced recoveries when applied to the analysis of preservatives such as insecticides in wood and wood-based materials. This is especially true in the presence of plastic or resin based adhesives or coatings in or on the wood and wood-based materials.
Immunoassays such as enzyme linked immunosorbent assays are presently used for the analysis of pesticides on wood, vegetables and surface treated seeds. The use of immunoassay techniques using conventional immunoassay methodology in an effort to analyse the amount of insecticide infused into wood-based materials has revealed that these techniques are inadequate for infused insecticides due to the low recoveries.
The term "preservative" is understood to include not only the original active ingredient contained within the timber treatment formulation but also biologically active derivatives of the active ingredient that may arise during the timber treatment process or during the lifetime of the treated product.
Spec465(comp - revised) 3 31 March 2005 27^07 2007 08:26 FAX 04 6 3590198 DON HOPKINS •» IPONZ @002 Summary of the Invention It is therefore an object of the present invention to provide a method for determining biocides within wood wherein a high recovery is achieved.
Broadly in one aspect the invention consists of a method for quantitation of chemical preservatives used to treat wood, wood-based products and engineered wood products characterised in the use of chromatographic extraction methods combined with an enzyme linked immunosorbent assay comprising the steps of, particle size reduction of the wood-based material, soaking of the wood particles in a solvent, separation of the solvent from the wood particles and filtration of the solvent, dilution of the solvent into an aqueous medium and an analysis of the chemical preservative by enzyme linked immunosorbent assay.
The present invention is based on the surprising discovery that when aspects of the immunoassay technology are combined with aspects of chromatography analyses when applied to the analysis of preservatives in wood and wood-based materials, a very high recovery is obtained.
Surprisingly, the invention in this form yields high rates of extraction of imidacioprid relative to conventional methodology for both high performance liquid chromatography and immunoassay techniques. 4 INTELLECTUAL PROPERTy OFFICE OF N2. 2 7 JUL 2007 Description of the Preferred Embodiment of the Invention According to a preferred form of the invention the method includes the steps of reducing the particle size, through mechanical means of the wood, wood-based material or engineered wood product to be extracted, using organic liquids that can penetrate the wood matrix as extraction solvents, filtration of extracts and preparation of standards using appropriate untreated wood extracts.
Preferably the particle size of the wood-based material being analysed is reduced to between 1000 and 10 micrometres diameter or less. The reduction in particle size can be carried out before extraction solvent using a Wiley mill or after extraction solvent is added using an industrial type high shear blender like a Silverson_.
The extraction solvent is generally an organic solvent such as, but not restricted to, methanol, dichloromethane, acetone, or toluene. Non water miscible solvents are then stripped from the extract by evaporation under reduced pressure and taken into either water or methanol prior to analysis with ELISA techniques. Water miscible solvents can be used providing they are diluted into water by a ratio of 400:1 or greater.
The filtration of extracts can involve filtration with .02 micrometre pore filters.
Spec465(comp - revised) 31 March 2005 The preparation of standards of known concentration using extracts from appropriate untreated wood-based materials can be in accordance with techniques known within the art.
According to a further embodiment of the invention accelerated solvent extraction, and soxhlet extraction can also be used.
More particularly a preferred embodiment of the invention includes the following steps. a) Primary mechanical fragmentation of the treated wood, wood-based product or engineered wood product. b) Suspension of the wood particles in an appropriate extraction solvent. c) Secondary fragmentation of the suspended wood particles in order to reduce particle size. d) Incubation of the suspended wood particles. e) Separation of the extraction solvent from suspended wood solids. f) Dilution of the extraction solvent into a suitable aqueous sample buffer.
Spec465(comp - revised) 6 31 March 2005 g) Determination of the concentration of extracted and diluted preservative using an enzyme-linked immunosorbent assay directed at the preservative of interest.
Primary mechanical fragmentation of the wood product (step a above) may include but is not restricted to milling, grinding, shaving, shredding, or sanding or a combination of the above, and may be achieved using equipment such as a Willey mill, or a Silverson as disclosed above.
The extraction solvent used in step b above in the preferred form of the inventions is able to both penetrate the wood matrix and solubilise the preservative of interest. Accordingly the solvent may include various organic solvents, water, or aqueous mixtures containing solubility aids such as salts, detergents, or a combination thereof.
Secondary mechanical fragmentation of the suspended wood particles (step c above) may include but is not restricted to shearing in an in-line or batch type high shear mixer, treatment with ultrasound, rapid pressurisation and depressurisation as in a French press or a Manton Gaulin mixer, other methods of homogenisation known to those skilled in the art, or a combination of treatments.
Spec465(comp - revised) 7 31 March 2005 Incubation of the suspended wood particles (step d above) is in the preferred form of the invention sufficient to allow equilibration of the preservative of interest between the solid and liquid phases of the extraction mixture. It is to be noted that during the incubation the mixture may be stirred, heated, treated with ultrasound, subjected to one or more freeze-thaw cycles, evacuated, pressurised, or a combination of these treatments, in order to facilitate diffusion of the preservative.
Separation of the extraction solvent and soluble compounds from the wood solids (step e above) may be achieved by centrifugation, screening, sieving, decantation, or filtration. Preferably the extraction solvent is separated by centrifugation and filtration through a 0.2 micron filter.
In order to be quantitated by ELISA technique the extracted preservative is preferably presented in a predominantly aqueous phase. The extraction solvent containing the preservative of interest may be diluted directly into a suitable aqueous sample buffer in the case of a water miscible solvent (step f above), or in the case of a non-water miscible solvent, the solvent may be removed by evaporation and the preservative re-dissolved in the sample buffer.
Suitable aqueous sample buffers include water or, preferably, a buffered saline solution containing additional compounds as "blocking agents" intended to reduce non-specific binding reactions in the ELISA. Examples include phosphate-buffered saline or tris-buffered saline, containing in addition one or more detergents, Spec465(comp - revised) 8 31 March 2005 proteins, or synthetic polymers, in concentrations and combinations known to those skilled in the art. It should be noted that these blocking agents may be included in the aqueous sample buffer or may be added at a later stage during execution of the ELISA.
Examples The following example relates to the analyses of commercially manufactured and treated sheets of laminated veneer lumber made of pinus radiata veneers and cured with phenol-formaldehyde resin for the amount of imidacloprid present per one hundred grams of oven dried wood sample.
Spec465(comp - revised) 9 31 March 2005 Example 1.
Sample code Method of extraction and cleanup Method of analysis Average recoveries <40% w/w Average recoveries >40% w/w ETS 295 Presently accepted method.
HPLC with UV detection.
X ETS 295 Acidified alcohol with dual column SPE cleanup.
HPLC with MS detection.
X ETS 295 Ester extraction with GPC cleanup.
HPLC with MS detection.
X ETS 295 Accelerated solvent extraction with acidified alcohol.
HPLC with UV detection.
X ETS 285#1 Soxhlet extraction with ketone.
HPLC with UV detection.
X ETS 285#1 Soxhlet extraction with haloalkane.
HPLC with UV detection.
X ETS 295 Extraction with acetonitrile and derivitised with NBTA.
GC with MS detection.
X ETS 295 Extraction with haloalkane and derivitised with NBTA.
GC with MS detection.
X ETS 295 Extraction with acetonitrile and derivitised with HFBA.
GC with MS detection.
X ETS 295 Extraction with haloalkane and derivitised with HFBA.
GC with MS detection.
X ETS 295 Extracted with alcohol enzyme linked immunosorbent assay X Spec465(comp - revised) 31 March 2005 Thus the present invention provides a method of determining biocides in wood, wood-based products and wood engineered products where the method links extraction techniques most commonly employed in GC and HPLC type techniques for analysing compounds in wood, then using ELISA techniques to analyse these extractants. Thus there is a solvent (non-water miscible) extraction technology followed by the water miscible analysis technology. In the past there has been no attempt to employ ELISA form of analysis to wood extractions due to the nature of the solvents used in extraction. The present invention, therefore, employs the more powerful extraction techniques of solvents, but then by evaporating the solvent moving to a water system where the extractant is analysed via a water miscible system.
According to the present invention therefore a recovery higher than normal methods of analysis is achieved when immunoassay technology is combined with aspects of chromatographic analyses. Thus, analysis of insecticides in wood and wood-based materials when low dosages of insecticide have been applied can nevertheless yield surprisingly high rates of extraction. Therefore, the present invention provides a method for determining biocides within wood which represents a useful and surprising advance in the art.
Spec465(comp - revised) 11 31 March 2005 26/07 2007 15:22 FAX 64 6 3590198 DON HOPKINS ■+ IPONZ 11003 12

Claims (17)

WHAT WE CLAIM IS:-
1. A method of quantitation of chemical preservatives within wood, wood-based products and engineered wood products characterised in the use of chromatographic extraction methods combined with an enzyme linked immunosorbent assay comprising the steps of: I a) particle size reduction of the wood-based material b) soaking of the wood particles in a solvent c) separation of the solvent from the wood particles and filtration of the solvent d) dilution of the solvent into an aqueous medium e) analysis of the chemical preservative by enzyme linked immunosorbent assay.
2. The method according to claim 1 wherein the particle size of the wood-based material being analysed is reduced to between 1000 and 10 micrometres diameter.
3. The method according to claim 1 or 2 wherein the extraction solvent is a substantially organic solvent.
4. The method according to any one of claims 1 to 3 wherein the filtration of extracts includes filtration with 0.02 micrometre pore filters.
5. The method according to any one of claims 1 to 4 wherein accelerated solvent extraction, and soxhlet extraction is used. INTELLECTUAL PROPERTY OFFICE OF N.Z. 2 6 JUL 200? RECEIVED 26/07 2007 15:22 FAX 64 6 3590198 DON HOPKINS -» IPONZ 1004 13 7. 11.
The method according to any one of claims 1 to 5 wherein the reduction of particle size is by a primary mechanical fragmentation step carried out by one or more of milling, grinding, shaving, shredding or sanding.
The method according to any one of claims 1 to 6 further including a secondary mechanical fragmentation step carried out in the presence of organic solvent by one or more of shearing in an in-line or batch type high shear mixer, ultrasound, rapid pressurisation or depressurisation or other methods of homogenisation, preferably in-line high shear mixing.
The method according to any one of claims 1 to 7 further including incubation of suspended wood particles resulting from particle size reduction, sufficient to achieve equilibration of the preservative of interest between solid and liquid phases,
The method according to claim 8 wherein during incubation the mixture is stirred, heated, treated with ultrasound, subjected to one or more of freeze-thaw cycles, pressurised or a combination of any of these treatments in order to facilitate diffusion of the preservative.
The method according to any one of claims 1 to 9 wherein separation of the extracted solvent and soluble compounds from wood solids is achieved by centrifugation, screening, sieving, decantation or filtration-
The method according to claim 10 wherein the extraction solvent is separated by centrifugation and filtration through a fitter of substantially 0.2 micron.
The method according to any one of claims 1 to 11 wherein the extracted preservative is presented in a predominantly aqueous phase for execution of the ELISA. INTELLECTUAL PROPERTY OFFICE OF N.Z. 2 6 JUL 2007 26/07 2007 15:22 FAS 64 6 3590198 DON HOPKINS -» IPONZ @005 14
13. The method according to claim 12 wherein the extraction solvent containing the preservative is diluted directly into an aqueous buffer.
14. The method according to claim 13 wherein the aqueous buffer is a buffered saline solution containing blocking agents.
15. The method according to claim 14 wherein the buffer is phosphate-buffered saline or tris-buffered saline and one or more detergents, proteins or synthetic polymers as blocking agents.
16. The method according to claim 14 or 15 wherein the blocking agents are included in the aqueous sample buffer or added at a later stage during execution of the ELISA
17. The method according to any one of claims 1 to 16 substantially as herein described with reference to the Example. GEORGE WILLIAM MASON, JOHN BRODIE MATTHEWS, JOHN SUTHERLAND AULD, PETER JAMES HAYWARD, CHRISTINE ANNE HAYWARD trading in Partnership as TAPUAE PARTNERSHIP By their Attorneys DON HOPKINS & ASSOCIATES Per: INTELLECTUAL PROPERTY OFFICE OF N.Z. 2 6 JUL 2007 RECEIVED END
NZ53215104A 2004-04-06 2004-04-06 A method of quantitation of chemical preservatives within wood using enzyme linked immunosorbent assay technology combined with chromatographic analysis NZ532151A (en)

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NZ53215104A NZ532151A (en) 2004-04-06 2004-04-06 A method of quantitation of chemical preservatives within wood using enzyme linked immunosorbent assay technology combined with chromatographic analysis
AU2005201412A AU2005201412B2 (en) 2004-04-06 2005-04-05 Method For Determining Biocides Within Wood

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NZ53215104A NZ532151A (en) 2004-04-06 2004-04-06 A method of quantitation of chemical preservatives within wood using enzyme linked immunosorbent assay technology combined with chromatographic analysis

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AU2005201412B2 (en) 2010-03-04

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