EXTRUDATES COMPRISING VITAMIN B9

Abstract

The present invention relates to extrudates which comprise folic acid. To increase storage stability a solid pH buffer is added. Such extrudates have a long shelf-life even if the extrudates comprise in addition to folic acid vitamin B1 and/or vitamin B2.

Claims

1. Extruded strand, wherein said extruded strand comprises vitamin B9, at least one pH buffer, at least one filler and water.

2. Extruded strand according to claim 1, wherein said pH buffer is solid at room temperature and wherein said pH buffer is preferably a mixture of (i) ascorbic acid and (ii) an edible salt of ascorbic acid.

3. Extruded strand according to claim 1, wherein said extruded strand comprises at least one further micronutrient and wherein said at least one further micronutrient is preferably selected from the group consisting of minerals, fat-soluble vitamins, water-soluble vitamins, amino acids, polyunsaturated fatty acids and carotenoids.

4. Extruded strand according to claim 1, wherein said extruded strand comprises at least one further water-soluble vitamin preferably selected from the group consisting of vitamin B1 and vitamin B2.

5. Extruded strand according to claim 1, wherein said extruded strand comprises from 15 weight-% to 60 weight-% water, preferably from 20 weight-% to 55 weight-% water and more preferably from 25 weight-% to 45 weight-% water, based on the total weight of the extruded strand.

6. A plurality of extrudates, wherein the extrudates are obtainable by cutting the extruded strand according to claim 1, and wherein said cutting is optionally followed by spheronization.

7. Plurality of extrudates obtainable by drying the extrudates of claim 6, wherein the extrudates comprise preferably less than 10 weight-% water, more preferably less than 8 weight-% water and most preferably less than 5 weight-% water, based on the total weight of said extrudates.

8. Plurality of extrudates according to claim 7, wherein the pH of a liquid obtainable by dispersing 1 g of the extrudates in 40 ml deionised water is at room temperature from 4.6 to 6, preferably from 4.65 to 5.2 and more preferably from 4.7 to 5.

9. Plurality of extrudates according to claim 7, wherein the vitamin B9 content of the extrudates is after 3 months storage in a closed aluminium bag at 30° C. and 65% humidity at least 70%, preferably at least 75% and most preferably at least 80% of the vitamin B9 content of said extrudates before storage.

10. Food, feed or instant powder comprising a plurality of extrudates according to claim 6, wherein said instant powder is suitable for preparing a beverage.

11. Method of manufacturing a plurality of extrudates, wherein a composition comprising vitamin B9, at least one pH buffer, at least one filler and water is extruded.

12. Method according to claim 11, wherein the temperature at the die of the extruder is from 50° C. to 120° C., preferably from 55° C. to 90° C. and more preferably from 60° C. to 80° C.

13. Method according to claim 11, wherein the die of the extruder has at least one hole, and wherein the diameter of said hole is preferably from 0.1 mm to 2 mm, more preferably from 0.3 mm to 1.2 mm and most preferably from 0.4 mm to 0.8 mm.

14. Use of a pH buffer to increase shelf-life of an extrudate which comprises vitamin B9.

15. Use according to claim 14 or method according to claim 11, wherein said pH buffer is solid at room temperature and wherein said pH buffer is preferably a mixture of (i) ascorbic acid and (ii) an edible salt of ascorbic acid, and wherein said edible salt of ascorbic acid is preferably sodium ascorbate.

Description

FIGURES

[0046] FIG. 1 shows the result of Example 3. The relative content of vitamin B9 in the extrudates of Example 1 was measured after extrusion (time point: 0 month), and after 1 month, 2 months and 3 months storage time. On the y-axis, the measured vitamin B9 content is indicated in percentage of the calculated vitamin B9 content. Example: 90% vitamin B9 per se stability means that 10% of vitamin B9 which was used to manufacture the extrudates is no longer present.

[0047] Extrudate #132 has higher vitamin B9 per se stability than the other extrudates. Extrudate #132 comprises the pH buffer of the invention.

[0048] FIG. 2 shows a plurality of extrudates after drying and without spheronization. The individual extrudates have a diameter between 0.5 mm and 2 mm. The plurality of extrudates resembles a coarse powder and is flowable.

EXAMPLES

Example 1 (Manufacturing of Extrudates Comprising Folic Acid)

[0049] Extrudates #132 were manufactured as follows:

[0050] A powder containing folic acid, a pH buffer (ascorbic Acid and sodium ascorbate), a vitamin mix (vitamins B1, B2, B6, B3 and B12), a filler (wheat starch and durum wheat semolina) and optionally a lubricant 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 6 (electrically heated and water-cooled) barrels and a die head (12 or 21×0.5 mm) with a screw diameter of 16 mm and a length to diameter ratio of 40. Deionised water was injected into the second barrel. The temperature of barrels 2-6 as well as the die head was allowed to reach adiabatic extrusion conditions. The powder premix was fed at 500 g/h and 60 g/h water was added. Strands were then extruded. To obtain a plurality of extrudates, the extruded strands were directly die-face cut by two rotating knives at the die head. After die-face cutting the solid extrudates 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 weight-%, based on the total weight of said extrudates.

[0051] Extrudates #133, #131 and #124 were manufactured in the same manner as extrudates #132. The exact composition of all extrudates is shown in below TABLE 1.

TABLE-US-00001 TABLE 1 Extrudates Extrudates Extrudates Extrudates #132 #133 #131 #124 ingredient weight-% weight-% weight-% weight-% Folic Acid 0.08 0.08 0.08 0.27 Sodium 11.35 — 15.12 — Ascorbate Ascorbic Acid 3.76 15.12 — — Vitamin mix 5.02 4.73 5.02 15.73 filler 73.79 74.07 73.78 77 Lubricant 6 6 6 7

[0052] In above TABLE 1, weight-% refers to the total weight of the respective extrudates, not including any residual water. The vitamin mix was identical for all extrudates and comprised thiamine mononitrate (vitamin B1), riboflavin (vitamin B2), pyridoxine hydrochloride (vitamin B6), niacinamide (vitamin B3) and crystalline vitamin B12. The filler and the optional lubricant was also identical for all extrudates.

Example 2 (pH Measurement)

[0053] The pH of extrudates #132 was measured as follows:

[0054] A plurality of extrudates #132 having a total mass of 1 g was added to 40 ml deionised water at room temperature and allowed to stir for 1 h to ensure all extrudates were dispersed. The pH was then measured using a Metrohm 744 pH meter.

[0055] The pH of extrudates #133, #131 and #124 was measured in the same manner as the pH of extrudates #132. The result of these measurements is indicated in below TABLE 2.

TABLE-US-00002 TABLE 2 Example Extrudate pH buffer pH 1 #132 ascorbic acid and sodium ascorbate 4.73 2 #133 ascorbic acid only 3.7 3 #131 sodium ascorbate only 6.25 5 #124 no ascorbic acid 4.51 no sodium ascorbate

Example 3 (Storage Stability)

[0056] The relative content of vitamin B9 in extrudates of Example 1 was measured after extrusion (time point: 0 month), and after 1 month, 2 months and 3 months storage time. Storage conditions: 30° C., 65% humidity, in closed aluminium bags.

[0057] The following method was applied:

[0058] 2 g of the respective extrudates was weighed into a volumetric flask and allowed to dissolve at pH 7 in mobile phase at pH 7. After a set period of time, an aliquot (10 μl) was injected onto a Nucleosil 100-7 C18 (Macherey & Nagel) column connected to an Agilent HPLC system equipped with a UV/VIS detector. Mobile phase consisted of 13.5% Acetonitrile and 86.5% 0.25N pentasulfonate/0.25N heptasulfonate Na and was kept at a constant flow rate of 1.4 ml min.sup.−1. Vitamin B9 was detected at a wavelength of 290 nm and the area of the signal was calculated using a standard graph.

[0059] The results of the measurement are shown in FIG. 1. FIG. 1 shows that less vitamin B9 decomposes during storage if the pH buffer system of the invention had been added to the composition which was extruded.