POUCHED PRODUCT FOR ORAL USE COMPRISING WATER INSOLUBLE SUBSTRATE PARTICLES

Abstract

Described is a pouched product for oral use that includes a liquid permeable pouch and a nicotine containing filling material enclosed by the pouch, wherein the filling material is a tobacco free filling material or includes tobacco material in an amount of at most 10% by total weight of the filling material; has a pre-use moisture content of from 1% to 35% by total weight of the filling material; contains nicotine in an amount of from 0.5% to 2% by total weight of the filling material; and comprises water insoluble substrate particles and one or more water-soluble components; wherein the water insoluble substrate particles are ball-shaped particles constituting at least 65% by dry weight of the filling material, the water insoluble substrate particles having a d50 particle size of from 0.25 mm to 2.0 mm.

Claims

1. A pouched product for oral use comprising a liquid permeable pouch and a nicotine containing filling material enclosed by the pouch, wherein the filling material is a tobacco free filling material or comprises tobacco material in an amount of at most 10% by total weight of the filling material; has a pre-use moisture content of from 1% to 35% by total weight of the filling material; contains nicotine in an amount of from 0.5% to 2% by total weight of the filling material; and comprises water insoluble substrate particles and one or more water-soluble components; wherein the water insoluble substrate particles are ball-shaped particles constituting at least 65% by dry weight of the filling material, the water insoluble substrate particles having a d50 particle size of from 0.25 mm to 2.0 mm.

2. A pouched product according to claim 1, wherein the water insoluble substrate particles have a d50 particle size of from 0.25 mm to 1.5 mm.

3. A pouched product according to claim 2, wherein the water insoluble substrate particles have a d50 particle size of from 0.25 mm to 1.0 mm.

4. A pouched product according to claim 3, wherein the water insoluble substrate particles have a d50 particle size of from 0.25 mm to 0.6 mm.

5. A pouched product according to claim 1, wherein the water insoluble substrate particles have a d50 particle size of from 0.3 mm to 2.0 mm.

6. A pouched product according to claim 5, wherein the water insoluble substrate particles have a d50 particle size of from 0.3 mm to 1.5 mm.

7. A pouched product according to claim 6, wherein the water insoluble substrate particles have a d50 particle size of from 0.3 mm to 1.0 mm.

8. A pouched product according to claim 7, wherein the water insoluble substrate particles have a d50 particle size of from 0.3 mm to 0.6 mm.

9. A pouched product according to claim 1, wherein the water insoluble substrate particles have a d50 aspect ratio of 0.8 or above and a d50 sphericity of 0.8 or above.

10. A pouched product according to claim 1, wherein the water insoluble substrate particles comprise or consist of particles of microcrystalline cellulose, water insoluble starch, silica, or a mixture thereof.

11. A pouched product according to claim 10, wherein the water insoluble substrate particles comprise particles of microcrystalline cellulose.

12. A pouched product according to claim 1, wherein the water insoluble substrate particles constitute 75% by dry weight to 95% by dry weight of the filling material.

13. A pouched product according to claim 1, wherein the water insoluble substrate particles contain less than 0.5% by weight of particles passing through a sieve having a mesh size of 250 m.

14. A pouched product according to claim 1, wherein the filling material contains less than 0.5% by weight of particles passing through a sieve having a mesh size of 250 m.

15. A pouched product according to claim 1, wherein the water insoluble substrate particles have a narrow particle size distribution.

16. A pouched product according to claim 1, wherein the filling material contains at most 15% by dry weight of the filling material of sugar alcohol.

17. A pouched product according to claim 1, wherein substantially all nicotine in the filling material is located on an outer surface of the water insoluble substrate particles.

18. A pouched product according to claim 1, wherein a filling degree of the liquid permeable pouch is 80% or less.

19. A pouched product according to claim 1, wherein the liquid permeable pouch is formed from a nonwoven material, such as a nonwoven material comprising staple fibres of regenerated cellulose.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0075] The present invention will be further explained hereinafter by means of non-limiting examples and with reference to the appended drawings wherein:

[0076] FIG. 1 shows a pouched product for oral use;

[0077] FIG. 2 shows a portion of a filling material in the pouched product of FIG. 1;

[0078] FIG. 3 shows test equipment for use when determining filling degree of an oral pouched product; and

[0079] FIG. 4 shows a schematical view of an image analysis instrument.

DETAILED DESCRIPTION

[0080] The pouched product 1 for oral use which is shown in FIG. 1 comprises a liquid permeable cover material 2 and a portion sized amount of a filling material 3 comprising a plurality of water insoluble substrate particles 4 enclosed by the liquid permeable cover material 2. The cover material 2 may be any suitable type of cover material as disclosed herein and is formed into a generally rectangular pouch into which the filling material 3 has been inserted.

[0081] A common way of making a pouched product having a generally rectangular pillow-like shape, such as the pouched product 1 shown in FIG. 1, is either to provide the cover material as a seamless and endless tube or to form a flat web of cover material into an endless tube which is provided with a continuous seal in the longitudinal direction of the endless tube. The endless tube is subsequently intermittently sealed in the transverse direction of the endless tube while filling the endless tube with filling material into pockets which are created between the transverse seals. Individual pouched products are severed from the filled and sealed tube of cover material and are usually packed in user containers. Sealing of the cover material may be made with any suitable method or combination of methods, such as by means of adhesive, heat sealing, ultrasonic welding, needling, etc. Heat sealing and ultrasonic welding require the cover material to contain at least a functional amount of thermoplastic material, such as thermoplastic fibres or thermoplastic binders.

[0082] The longitudinal seal created during manufacturing appears as a longitudinal seal 6 extending along the length l of the pouched product 1 shown in FIG. 1. No such seal will be present if the cover material is provided in the form of an endless seam-less tube. The transverse seals form end seals 7 which define the width w of the pouched product 1. The pouched product 1 has a first main surface 8 and a second main surface 9 and a thickness t being defined as the greatest perpendicular distance between the first main surface 8 and the second main surface 9.

[0083] The particles 4 of the water insoluble particulate material may constitute a very high proportion of the total dry weight of the filling material 3, such as 65% by dry weight to 99% by dry weight of the filling material, as set out herein.

[0084] The filling material 3 further comprises one or more water soluble components 11, such as flavours, sweeteners, active ingredients such as nicotine, etc. as disclosed herein.

[0085] A part of a filling material 3 for an oral pouched product as disclosed herein is shown in FIG. 2, the filling material 3 comprising a plurality of generally spherical, ball-shaped, water insoluble substrate particles 4 having a thin layer of water soluble components on the surfaces of the particles 4.

[0086] As set out herein, the particles 4 of the filling material have a relatively large d50 particle size within the range of from 0.25 mm to 2.0 mm.

[0087] FIG. 2 shows only a very small number of particles 4. In a full portion of filling material 3 for an oral pouched product 1, the number of particles 4 in the water insoluble particulate material is considerably higher, such as in the order of 150 particles or more which means that a large majority of the particle surfaces will be located in the interior of the filling material 3.

Test Methods

Method for Determining Moisture Content, Loss On Drying, LOD

[0088] The moisture content as referred to herein may be determined by using a method based on literature references Federal Register/vol.74, no. 4/712-719/Wednesday, Jan. 7, 2009/Notices Total moisture determination and AOAC (Association of Official Analytical Chemics), Official Methods of Analysis 966.02: Moisture in Tobacco (1990), Fifth Edition, K. Helrich (ed). In this method, the moisture content is determined gravimetrically by taking 2.50.25 g sample and weighing the sample at ambient conditions, herein defined as being at a temperature of 22 C. and a relative humidity of 60%, before evaporation of moisture and after completion of dehydration. Mettler Toledo's Moisture Analyzer HB43, a balance with halogen heating technology, is used (instead of an oven and a balance as in the mentioned literature references) in the experiments described herein. The sample is heated to 105 C. (instead of 99.50.5 C. as in the mentioned literature references). The measurement is stopped when the weight change is less than 1 mg during a 90 second time frame. The moisture content as weight percent of the sample is then calculated automatically by the Moisture Analyzer HB43.

Method for Determining Particle Size and Particle Shape by Image Analysis

[0089] Particle roundness, particle sphericity, aspect ratio, and particle size were determined using a QicPic image analysis instrument from 2012, Sympatec GmbH, ID No. 290-D, with Rodos/L dispersion line ID NO 214D and Vibri/L sample feeding ID NO 273, or equivalent equipment. A well dispersed particle flow is led through the image plane of the instrument, as shown in FIG. 4 where 21 is a pulsed light source, 22 is a beam expansion unit adaptable to measuring range, 23 is a dispersing unit, 24 is a particle flow, 25 is a lens and 26 is a camera. If the particles are small, a high number of particles per image frame may be captured, such as in the order of 50,000 to 100,000 particles per image frame. For larger particles, such as particles having a particle size from 300 m to 3000 m, the number of particles per image frame may be substantially less and may be in the order of from 300 to 2000 particles per image frame.

Sieving Method

[0090] A commercially available particle screening equipment such as a Retsch/AS 200 control vibrating sieve may be used. A 10 g sample of the tested filling material or water insoluble substrate particles is placed on the sieve such as a sieve having a mesh size of 250 m and is vibrated for 1 minute with an amplitude of 1 mm.

[0091] The weight of the upper fraction and the lower fraction is measured for the sample and the weights are used for calculating the proportion of the sample which has passed through the mesh.

Method for Determining Filling Degree in an Oral Pouched Product

[0092] The measurements are carried out at ambient conditions, as defined herein. The pouches 1 are applied in a frame 20 shown in FIG. 3 with a first transverse end seal 7 placed below a second transverse end seal 7. The pouches 1 are attached to the frame 20 by means of a double-sided tape applied to the first transverse end seal 7. The frame 20 is designed to support the filled pouch 1 without compressing it. Following application of the filled pouch in the frame, the shortest distance between the upper surface of the filling material 3 and the first transverse seal 7, i.e., the height of the filling material 3 in the pouch 1, is determined using a digital tabletop caliper device having a resolution of 0.01 mm. A background LED light may be directed at the pouch 1 for improving content discernability. Care should be taken not to agitate or shake the filled pouch 1 during application of the pouch in the frame.

[0093] The filling degree of the oral pouched product is calculated by dividing the measured height of the filling material in the pouch with the inner distance between the first and second transverse end seals 7, 7 and is reported in percent (%) of the available filling height.

Example

Sample Preparation

[0094] Five different MCC materials were tested as set out in Table 1.

TABLE-US-00001 TABLE 1 Example 1 Vivapur MCC spheres 700 supplied by JRS Pharma, Germany Example 2 Cellets 350 supplied by Pharmatrans, Switzerland Reference 1 Avicel PH-200 supplied by JRS Pharma, Germany Reference 2 Cellets 100 supplied by Pharmatrans, Switzerland Reference 3 Crushed particles of Example 1. The particles were crushed by means of milling in a mortar during 3 minutes until the particles had formed a fine powder.

[0095] The tested materials according to Examples 1 and 2 and References 1 and 2 had a sphericity, aspect ratio and particle size as set out in Table 2 when measured at d50 with the image analysis instrument from Sympatec GmbH. The materials according to Examples 1 and 2 contained less than 0.5% by weight of particles passing through a sieve having a mesh size of 250 m.

TABLE-US-00002 TABLE 2 Example 1 Example 2 Reference 1 Reference 2 Sphericity 0.817 0.804 0.810 0.842 Aspect ratio 0.962 0.913 0.742 0.875 Particle size 890 445 205 163 (m)

[0096] For each sample, a solution was prepared from 48.3 grams of 20% nicotine in glycerine (supplied by CNT, Germany), 6.5 grams of potassium carbonate, 15 grams of sodium chloride, 1 gram of acesulfame K and 110.3 grams of water.

[0097] The nicotine-containing solution was then mixed with 809 g grams of the MCC material to be tested and 10 grams of peppermint flavor. The mixture was allowed to rest for 16 hours at room temperature without stirring resulting in nicotine containing particles.

[0098] The particles of the 5 different sample materials were then packed in rectangular pouches as shown in FIG. 1 and having a width, w, of 12.5 mm and a length, l, of 37 mm. The inner length of the pouch between the end seals 7 was 32 mm. Each pouch was filled with nicotine containing particles to a filling degree of approximately 65.6%.

[0099] The pouch material which was used for all samples was a standard viscose nonwoven No. Z8732 from TENOWO GmbH.

Test Procedure

[0100] Seven test persons were each given 5 containers with two sample products containing one of the tested filling materials in each container, in total 10 sample products per test person. The test persons were also given 10 glass vials for storing the samples after use. Each vial was labelled with the sample to be put in the vial, e.g., Example 1, 10 minutes, Reference 3, 30 minutes, etc.

[0101] The test persons were instructed not to use any tobacco product or other nicotine containing product for at least 30 minutes before each test and to rinse the mouth with water before the test. The test persons were instructed to use the sample products in the way they normally would, but not to ingest any food or drink during the test period.

[0102] The tests were performed by the test persons by: [0103] 1. Selecting a vial at random and checking the label to see which sample to put in the vial. [0104] 2. Taking out a sample from the container containing the samples according to the label on the vial. [0105] 3. Placing the sample under the lip and letting it remain there for 10 or 30 minutes depending on what is written on the label on the vial in which the sample is to be put after use. [0106] 4. After use of the sample product, carefully removing the sample product with a pair of tweezers, while avoiding squeezing the sample. [0107] 5. Placing the used sample product in the assigned glass vial. [0108] 6. Storing the glass vials in a freezer until all sample products had been used.

[0109] The used samples were then analyzed for nicotine content. Non-used samples were also analyzed to establish original nicotine content. It was found that the filling materials of Example 1 and Example 2 had a nicotine release profile such that more than 30% of the nicotine had been extracted after 10 minutes and more than 40% of the nicotine had been extracted after 30 minutes. The filling material of Example 2, with water insoluble ball-shaped MCC particles having a particle size (d50) of 445 m were found to have surprisingly good nicotine release properties, with approximately 40% of the nicotine having been released already after 10 minutes and more than 55% of the nicotine having been released after 30 minutes. The filling material with water insoluble ball-shaped MCC particles having a particle size (d50) of 890 m was also found to have good nicotine release properties with slightly more than 30% of the nicotine having been released after 10 minutes and more than 45% of the nicotine having been released after 30 minutes.

[0110] The reference samples all showed a considerably lower nicotine release after 10 minutes, with only Reference 2 reaching an acceptable level of nicotine release after 30 minutes.

[0111] The results are shown in Table 3, below.

TABLE-US-00003 TABLE 3 Sample 0 min 10 min 30 min 10 min 30 min Weight* Sample (mg) (mg) (mg) % % (g) Ex. 1 5.47 3.80 2.97 30.6 45.7 0.70 Ex 2 5.20 3.11 2.32 40.2 55.5 0.72 Ref. 1 2.60 2.02 1.78 22.4 31.7 0.35 Ref. 2 5.36 4.07 2.83 24.0 47.1 0.70 Ref. 3 4.39 3.64 3.03 17.0 31.0 0.60 *Including pouch material