Method for purification of lactose
View Patent ↗The present invention relates to improved methods of purification of sugars and in particular to a method of preparing lactose. A low purity lactose source such as whey is subjected to a first demineralization step involving either ion-exchange or the addition of divalent metal cations, followed by a second demineralization step where alcohol is added. The invention also relates to lactose produced by this method and products comprising lactose produced by this method.
1. A method for the production of crystalline lactose of pharmaceutical grade from clarified whey solution including the steps of:
(a) ultrafiltration of the clarified whey solution to obtain whey permeate;
(b) primary demineralisation of the solution from step (a) by treatment with about 0.014 to 0.025 M calcium chloride and/or calcium hydroxide;
(c) filtration or centrifugation of the solution from step (b) and, optionally, treatment of the solution with charcoal;
(d) concentration of the solution from step (c) to 20% to 60% total solids;
(e) secondary demineralisation by addition of ethanol to the solution from step (d) to a final concentration of about 60%;
(f) filtration or centrifugation of the solution from step (e);
(g) crystallisation of lactose from the solution from step (f);
(h) centrifugation of the solution from step (g) and removal of lactose crystals; and
(i) washing lactose crystals obtained in step (h) with an alcoholic solution containing between 0% and 20% water and drying the crystals.
2. The method according to claim 1 , wherein the concentration of the solution from step (c) is by nanofiltration and evaporation, or reverse osmosis.
3. An improved method for the preparation of lactose crystals of at least food grade standard from a lower purity lactose source, the improvement including the steps of:
(a) treating a solution containing lactose with about 0.014M to 0.025M divalent metal ions to remove a proportion of minerals contained in the solution; and
(b) treating the divalent metal ion-treated solution with alcohol at a concentration of about 25% to 75% total liquid volume to remove residual minerals from the solution.
4. A method of preparing high purity lactose from a lower purity lactose source including two demineralisation steps as follows:
(a) primary demineralisation by treatment with about 0.014M to 0.025M divalent metal ions to provide a lactose-containing solution and a mineral precipitate, and
(b) secondary demineralisation of the lactose-containing solution from step (a) including the addition of alcohol at a concentration of about 25% to 75% total liquid volume to precipitate further minerals from the solution.
5. The method according to claim 4 , wherein after step (b) lactose is crystallized from the solution by a crystallisation step, step (c).
6. The method according to claim 5 , wherein the crystallisation is carried out by a single step procedure.
7. The method according to claim 5 , wherein the crystallisation is carried out over a period of about 4 hours.
8. The method according to claim 5 , wherein the crystallisation is carried out over a period of about 2 hours.
9. The method according to claim 4 , wherein the lactose-containing solution from step (a) is concentrated to 20% to 60% total solids before step (b).
10. The method according to claim 4 , wherein the divalent metal ion is calcium, magnesium or barium.
11. The method according to claim 4 , wherein the divalent metal ion is calcium derived from calcium chloride or calcium hydroxide; magnesium derived from magnesium chloride; or barium derived from barium chloride.
12. The method according to claim 4 , wherein the alcohol is ethanol, methanol, isopropanol or propanol.
13. The method according to claim 12 , wherein the alcohol is ethanol.
14. The method according to claim 13 , wherein the ethanol is present at approximately 60% total liquid volume.
15. The method according to claim 4 , wherein the temperature of the divalent metal ion-treated solution and the alcohol is between 40° C. and 79° C.
16. The method according to claim 4 , wherein the temperature of the divalent metal ion-treated solution and the alcohol is about 78° C.
17. The method according to claim 5 , wherein the step (c) is carried out in alcohol.
18. The method according to claim 5 , wherein the step (c) is carried out in alcohol present at between 25% to 75% total liquid volume.
19. The method according to claim 5 , wherein the crystals formed in step (c) are washed with an alcohol solution containing between 0% and 20% water.
20. The method according to claim 4 , wherein the high purity lactose has less than 0.3% ash.
21. The method according to claim 4 , wherein the high purity lactose is pharmaceutical grade lactose with less than 0.1% ash.
22. The method according to claim 4 , wherein when clarified whey screened to remove cheese particles and centrifuged to remove fat is used as a lactose source, the divalent metal ion treatment of step (a) is preceded by an ultrafiltration step to obtain whey permeate.
23. The method according to claim 4 , wherein the divalent metal ion-treated solution from step (a) is treated with one or more absorbents.
24. The method according to claim 23 , wherein the absorbent is charcoal.
25. The method according to claim 23 , wherein the solution treated with one or more absorbents is concentrated by nanofiltration and evaporation prior to step (b).
26. The method according to claim 4 , wherein the high purity lactose is recovered by centrifugation and is further washed and dried.