Multivitamin extrudates

Abstract

This invention relates generally to multivitamin extrudates. Their production as well as their use.

Claims

1. A free-flowing powder of sphere-like particles having a size of 100-600 μm which contain no fat-soluble vitamins, wherein the particles are an extrudate of a composition which consists of: at least 8 wt. %, based on total weight of the extrudate, of multiple water soluble B vitamins, and a wheat carrier material consisting of a combination of wheat starch, durum wheat semolina, and optionally at least one auxiliary agent.

2. The free-flowing powder according to claim 1, wherein the multiple water soluble B vitamins are present in an amount of at least 8 wt. % to 95 wt. %, based on the total weight of the extrudate.

3. The free-flowing powder according to claim 1, comprising 8 wt. % to 80 wt. %, based on the total weight of the extrudate, of the multiple water soluble B vitamins.

4. The free-flowing powder according to claim 3, wherein the multiple water soluble B vitamins consists of at least three water soluble B vitamins and the wheat carrier material.

5. The free-flowing powder according to claim 1, wherein the multiple water soluble B vitamins consists of more than one B vitamin selected from the group consisting of vitamin B1, vitamin B2, vitamin B3, vitamin B5, vitamin B6, vitamin B7, vitamin B9 and vitamin B12.

6. The free-flowing powder according to claim 1, wherein the at least one auxiliary agent is selected from the group consisting of antioxidants, butylated hydroxytoluene (BHT), butylated hydroxyanisole (BHA), propyl gallate, tert.butyl hydroxyquinoline, ascorbic acid esters of a fatty acid, ethoxyquin, plasticisers, stabilisers, humectants, protective colloids, dyes, fragrances, minerals, fillers and buffers.

7. The free-flowing powder according to claim 1, wherein the at least one auxiliary agent is present in an amount from 0.1 to 92 wt. %, based on the total weight of the extrudate.

8. The free-flowing powder according to claim 1, wherein the wheat starch and the durum wheat semolina are present in the extrudate in a weight ratio of the wheat starch to the durum wheat semolina of 1:1.

9. Food, feed, pharma and/or personal care formulations or premixes for food, feed, pharma and/or personal care formulations comprising the free-flowing powder according to claim 1.

Description

EXAMPLES

Example 1: Extruded Multicomponent Particle Comprising all B Vitamins

(1) This example describes the production of solid, extruded particles comprising all B vitamins (thiamine, riboflavin, pyridoxine, niacin, folic acid and cobalamin). The powder premix containing the B vitamins as well as wheat starch and durum wheat semolina as carrier materials was gravimetrically fed (Brabender Technologie) into the first barrel of a laboratory-scale co-rotating twin screw extruder (Thermo Fisher Scientific, HAAKE Polylab OS with PTW16/40 OS twin screw extruder). The extruder consisted of 10 (electrically heated and water-cooled) barrels and a die head (12 or 21×0 0.5 mm) with a screw diameter of 16 mm and a length to diameter ratio of 40. Demineralized water was injected into the second barrel. The temperature of barrels 2-10 as well as the die head was set to 20° C. The powder premix was fed at 500 g/h and 60 g/h water was added. The extrudate strands containing the B vitamins were directly die-face cut by two rotating knives at the die head. After die-face cutting the solid particles were dried in a laboratory-scale fluid bed drier (Retsch TG 200) for 60 minutes at 50° C. to obtain a final water content of 6 wt %.

(2) The content of the dry extrudate particles is shown in Table 1. The Vitamin B2-5-phosphate content was measured by HPLC of the freshly produced extrudate and a recovery of 93% was found.

(3) TABLE-US-00001 TABLE 1 Composition of dry extrudate containing all B vitamins. Ingredient Content, wt % in dry extrudate Thiamine mononitrate (B1) 0.829 Riboflavin 5′-phosphate sodium (B2) 0.96 Pyridoxine hydrochloride (B6) 0.74 Niacinamide (B3) 7.28 Folic Acid (B9) 0.19 Vitamin B12 Crystalline 0.001 Wheat starch 45.00 Durum wheat semolina 45.00

Example 2: Extruded Multicomponent Particle Comprising Oil- and Water-Soluble Vitamins

(4) This example describes the production of solid, extruded particles comprising oil- (Vitamin A acetate, Vitamin D3, Vitamin E acetate) and water-soluble (Vitamin C, thiamine, riboflavin, pyridoxine, niacin, folic acid and cobalamin) vitamins. The production of solid, extruded particles comprising emulsified oil-soluble vitamins as well as water-soluble vitamins was conducted on the laboratory-scale co-rotating twin screw extruder described in Example 1. The emulsifier (modified food starch) as well as the filler (microcrystalline cellulose) were premixed with the water-soluble vitamins as shown in Table 2. This powder premix was gravimetrically fed into the first barrel of the twin screw extruder. Demineralized water was injected into the second barrel. The temperature of barrels 2-10 as well as the die head was set to 50° C. The oil-soluble vitamins Vitamin A acetate, Vitamin D3 crystalline, d,l-alpha-tocopheryl acetate (optionally with added antioxidant such as d,l-alpha tocopherol or butylated hydroxytoluene (BHT)) were molten and premixed at 70° C. (Table 3). This oily melt was injected into barrel 5 and mixed with the other components in the downstream barrels. The powder premix was fed at 750 g/h, the oily premix at 40 g/h and 210 g/h water was added. The extrudate strands containing the oil- and water-soluble vitamins were collected, let to cool down to room temperature and subsequently cut by a pelletizer (Thermo Fisher Scientific). The cut, solid particles were dried in a laboratory-scale fluid bed drier (Retsch TG 200) for 60 minutes at 50° C. to obtain a final water content of 5 wt %.

(5) TABLE-US-00002 TABLE 2 Composition of powder premix for extrusion of water- and oil-soluble vitamins. Ingredient Content, wt % in powder premix Thiamine mononitrate (B1) 0.51 Ribofiavin 5′-phosphate sodium (B2) 0.61 Pyridoxine hydrochloride (B6) 0.47 Niacinamide (B3) 4.61 Folic Acid (B9) 0.12 Vitamin B12 Crystalline 0.001 Ascorbic acid fine powder (C) 20.39 Modified food starch 29.32 Microcrystalline cellulose 43.969

(6) TABLE-US-00003 TABLE 3 Composition of oily melt for extrusion of water- and oil-soluble vitamins. Ingredient Content, wt % in oily melt Vitamin A acetate crystalline 7.30 Vitamin D3 crystalline 0.08 d,l-alpha-tocopheryl acetate (E) 91.62 d,l-alpha-tocopherol 1.00

(7) The content of the dry extrudate particles is shown in Table 4. The Vitamin B2-5-phophate, Vitamin A acetate as well as Vitamin D3 contents were measured by HPLC of the freshly produced extrudate and recoveries of 94%, 89% and 100% were found, respectively.

(8) TABLE-US-00004 TABLE 4 Composition of dry extrudate containing oil- and water-soluble vitamins. Ingredient Content, wt % in dry extrudate Thiamine mononitrate (B1) 0.482 Riboflavin 5′-phosphate sodium (B2) 0.577 Pyridoxine hydrochloride (B6) 0.445 Niacinamide (B3) 4.374 Folic Acid (B9) 0.114 Vitamin B12 Crystalline 0.001 Ascorbic acid fine powder (C) 19.35 Modified food starch 27.82 Microcrystalline cellulose 41.73 Vitamin A acetate crystalline 0.373 Vitamin D3 crystalline 0.004 d,l-alpha-tocopheryl acetate (E) 4.679 d,l-alpha-tocopherol 0.051

Example 3: Extruded Multicomponent Particle Comprising Oil-Soluble Vitamins

(9) This example describes the production of solid, extruded particles comprising oil-soluble (Vitamin A acetate, Vitamin D3, Vitamin E acetate) vitamins. The production of solid, extruded particles comprising emulsified oil-soluble vitamins was conducted on the laboratory-scale co-rotating twin screw extruder described in Example 1. The emulsifier (modified food starch) as well as the filler (microcrystalline cellulose) were premixed at a ratio 2:3. This powder premix was gravimetrically fed into the first barrel of the twin screw extruder. Demineralized water was injected into the second barrel. The temperature of barrels 2-10 as well as the die head was set to 50° C. The oil-soluble vitamins Vitamin A acetate, Vitamin D3 crystalline, d,l-alpha-tocopheryl acetate (optionally with added antioxidant such as d,l-alpha tocopherol or butylated hydroxytoluene (BHT)) were molten and premixed at 70° C. (Table 5). This oily melt was injected into barrel 5 and mixed with the other components in the downstream barrels. The powder premix was fed at 500 g/h, the oily premix at 73 g/h and 300 g/h water was added. The extrudate strands containing the oil- and water-soluble vitamins were collected and subsequently spheronized in batches of 250 g at 1900 rpm for 15 minutes (Gabler R-250). The spheronized, solid particles were dried in a laboratory-scale fluid bed drier (Retsch TG 200) for 60 minutes at 50° C. to obtain a final water content of 4 wt %.

(10) The content of the dry extrudate particles is shown in Table 6. The Vitamin A acetate as well as Vitamin D3 contents were measured by HPLC of the freshly produced extrudate and recoveries of 88% and 92% were found, respectively.

(11) TABLE-US-00005 TABLE 5 Composition of oily melt for extrusion of oil-soluble vitamins. Ingredient Content, wt % in oily melt Vitamin A acetate crystalline 7.30 Vitamin D3 crystalline 0.08 d,l-alpha-tocopheryl acetate (E) 91.63 d,l-alpha-tocopherol 0.99

(12) TABLE-US-00006 TABLE 6 Composition of dry extrudate containing oil-soluble vitamins. Ingredient Content, wt % in dry extrudate Vitamin A acetate crystalline 0.94 Vitamin D3 crystalline 0.01 d,l-alpha-tocopheryl acetate (E) 11.73 d,l-alpha-tocopherol 0.13 Modified food starch 34.87 Microcrystalline cellulose 52.32