Food or edible material: processes – compositions – and products – Involving ion exchange – sequestering or chelating material
Reexamination Certificate
1999-09-17
2001-06-19
Nessler, Cynthia L. (Department: 1761)
Food or edible material: processes, compositions, and products
Involving ion exchange, sequestering or chelating material
C426S599000, C426S616000, C426S615000, C426S422000, C426S424000, C210S660000, C210S670000, C210S673000, C210S692000, C210S269000
Reexamination Certificate
active
06248382
ABSTRACT:
The invention concerns a process for reducing the patulin concentration in fruit juices, apparatus suitable for such a purpose and to related methods and means.
Patulin 4-Hydroxy-4H-furo[3,2-c]pyran-2(6H)-one (See Formula 1) is a mycotoxin produced by certain species of the genera Aspegillus and Penicillium. It is common in fruit that is rotting prior to processing for juice production.
Penicillium expansum
, is one such fungus and it is responsible for decomposition of apples and other fruit.
Apples destined for processing into juice production frequently are pack house rejects, wind falls, weather damaged or from cold storage. The fruit is often stored in the open for extended periods before processing. The percentage of fruit with varying degrees of rot can be high and inevitably will contain patulin.
The United Kingdom Ministry of Agriculture, Fisheries and Food in its Food Surveillance Paper No. 36 (1993) “Mycotoxins “Third Report” indicates that
Penicillium expansum
which produces patulin is a common storage rot in a diverse range of product(e.g. apples, peaches, pears, bananas, pineapples, apricots, cherries and grapes). They indicate that for apple juices patulin levels are generally higher in cloudy juices than in clear juices (highest levels in their data showed as 434 &mgr;g/kg and 118 &mgr;g/kg respectively).
Mycotoxins are undesirable in food because of their toxicity to animals and potential toxicity to human beings. The toxic activity of patulin, its teratogenicity, carcinogenicity and mutagenicity is known and is of concern.
The Codex Alimentarius Commission as part of the United Nations joint FAO/WHO Food Standards Programme in their 28th Session (June 1997) in respect of patulin indicates a PMTDI (Provisional Maximum Tolerable Intake) of 0.4 micrograms per kilogram body weight per day (i.e. 0.4 &mgr;g/kg.bw/day).
Apple juice can occasionally be heavily contaminated) notwithstanding that apple juice generally (particularly single strength apple juice eg; 11.5° Brix) has patulin levels of below 50 &mgr;g/l (micrograms per liter).
We believe that lower recommendations (eg; to below 25 &mgr;g/kg of patulin) are now being considered.
We have found in some apple juice samples (where there is a significant use of windfall and/or rotting fruit) to be as high as 1500 &mgr;g/l. However apple juice more commonly contains patulin up to 200 &mgr;g/l. Nevertheless a significant task exists in meeting targets for patulin content.
Different active and passive processes for reducing the patulin level to below the arbitrary limits mentioned are known. It is known that adding ascorbic acid or sulfur dioxide destroys patulin. However the addition of sulfur dioxide is legally not allowed in commercial operations.
Patulin also degrades in time in stored juice. The gradual loss of patulin from juice on storage is not a practical solution to providing juice with acceptable patulin levels.
Alcoholic fermentation of fruit juice is also reported to destroy patulin.
Some grades of activated carbon are effective at adsorbing patulin from juice. Dosages in the range 1~2 g/l provide up to 80% patulin reduction. Activated carbon can be used commercially to reduce patulin from fruit juice, but it is difficult to handle and is an expensive consumable item. Activated carbon is not viable to regenerate and reuse. It also adds to the solids loading of the factory effluent creating environmental problems.
It is an object of the present invention to provide a commercially viable process and/or apparatus for reducing the patulin concentration in fruit juices. It also involves providing (e.g. regeneration procedures and the products of any such processes or procedures) related procedures, methods and means.
In a first aspect the present invention consists in a process for reducing the patulin content in a fruit juice which comprises or includes
(i) presenting the juice to a resin material having in abundance micropores of less than 20 Å minimum pore width (“mpw”) and at least a pore surface capable of retaining patulin by the forces of chemisorption (for example, van der Waal and London dispersion interactions), and
(ii) harvesting the juice with a reduced patulin content from step (i).
The adsorption of patulin onto the surface of the micropores of the resin is dependent upon the plurality of the surface matrix and orientation of the polar groups on the patulin molecule. The forces of chemisorption are likely provided by van der Waal and London dispersion interactions. The energy of chemisorption is very small and the patulin molecules are able to undergo lateral diffusion and conformational changes on surrounding surfaces. Therefore the chemisorption is best described as the physical attraction on to a chemically inert adsorption surface.
Preferably the resin has weak base functionality although non-functionaries yet wettable resins may be used.
Preferably said resin is substantially devoid of mesopores and macropores.
It is believed that the resin and its micropores is such that caustic soda is substantially ineffective in chemically converting the micropore held patulin to a more easily flushed out patulin derivative.
Preferably said process uses a resin having very high internal surface areas yet a low mercury intrusion characteristic.
Preferably said resin has a surface area of greater than 900 (eg; from 900 to 1500) m
2
/g (BET).
Preferably said surface area is from 1000 to 1500 m
2
/g (BET).
Preferably said resin has a mercury intrusion (d
50
,A) of less than 100.
Preferably said resin has micropores in abundance of less than 15 Å (mpw).
Preferably said resin is in the form of a bed of fibres, beads or granules.
Preferably said beads granules or fibres have a section of from 300 to 1600 microns across.
Preferably said resin is a styrene divinyl benzene network copolymer resin.
Preferably said resin has been hypercrosslinked whilst in the swollen state.
Preferably said resin has in abundance micropores of minimum pore width of from 5 to 2 Å (mpw).
Preferably the resin has been regenerated after a previous use in a similar patulin extraction process.
Preferably said regeneration has involved the conversion of the resin held patulin to a more easily flushed out derivative using ammonia or a volatile base.
Preferably said conversion has involved the at least substantially in situ generation of ammonia or a volatile base from a high pH solution in contact with the resin.
Preferably said regeneration has subsequently involved after flushing out of the patulin derivative(s) the presentation of an acid to the resin.
Preferably the juice is presented to the resin in the range of 20 or greater bed volumes prior to regeneration of the resin, the bed volume range being expressed in proportion to a real or notional single juice strength.
Preferably the juice is presented to the resin at a rate of from about 4 to about 10 bed volumes/hour.
Preferably the resin has been tertiary amine functionalised but is presented to the juice in an acid form as opposed to the free base form thereby reducing the uptake of juice acid during the presentation of the juice to the resin.
Preferably the resin provides a bed of depth of from 0.5 to 2.0 meters.
In a further aspect the present invention consists in apparatus for use in a process as previously defined, said apparatus having at least one vessel providing a bed of the resin and which is operable in at least two modes, the first mode being that which presents juice to and harvests juice from the resin and the second mode being that which regenerates the resin.
In still a further aspect the present invention consists in a method of regenerating a micropored resin which contains patulin in micropores which comprise or includes, in a high pH liquid environment containing the patalin fouled resin, generating a basic vapour (preferably ammonia) sufficient to convert the micropore held patulin to a more easily flushed out derivative or derivatives and thereafter flushing the derivative(s) from the micropores.
Preferably ammonia is generated
Lyndon Rex M.
Miller Chris J.
Bucher-Alimentech Ltd.
Burns, Doane, Swecker and Mathis, L.L.P.
Nessler Cynthia L.
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