# US 12,006,085 B2 · Fill-finish process for peptide solutions

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- Number: US 12,006,085 B2
- Document ID: US12006085B2
- Status: Granted
- Kind: B2
- Application number: 17/832,612
- Filed: 2022-06-04
- Published: 2022-10-13
- Granted: 2024-06-11
- Earliest claimed: 2012-07-06
- Assignees: 3-D Matrix, Ltd.
- Applicants: 3-D Matrix, Ltd.
- Inventors: Masahiro Nohara; Yuya Hasegawa
- Web page: https://patentgrep.com/patent/US12006085B2

## CPC

- B65B 55/12: Sterilising contents prior to, or during, packaging
- B65B 3/003: {Filling medical containers such as ampoules, vials, syringes or the like}
- B65B 55/04: Sterilising wrappers or receptacles prior to, or during, packaging {(sterilising bottles B67C7/00)}
- B65B 63/00: Auxiliary devices, not otherwise provided for, for operating on articles or materials to be packaged
- C07K 1/34: by filtration, ultrafiltration or reverse osmosis
- C07K 1/36: by a combination of two or more processes of different types
- C07K 7/08: having 12 to 20 amino acids (gastrins C07K14/595; somatostatins C07K14/655; melanotropins C07K14/68)
- A61K 38/00: Medicinal preparations containing peptides (peptides containing beta-lactam rings A61K31/00; cyclic dipeptides not having in their molecule any other peptide link than those which form their ring, e.g. piperazine-2,5-diones, A61K31/00; ergot alkaloids of the cyclic peptide type A61K31/48; containing macromolecular compounds having statistically distributed amino acid units A61K31/74; medicinal preparations containing antigens or antibodies A61K39/00; medicinal preparations characterised by the non-active ingredients, e.g. peptides as drug carriers, A61K47/00)
- C07K 5/101: {the side chain containing 2 to 4 carbon atoms, e.g. Val, Ile, Leu}
- C07K 5/1019: {with the first amino acid being basic}
- B65B: MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING (bundling and pressing devices for cigars A24C1/44; devices for tensioning and securing binders adapted to be supported by the article or articles to be bound B25B25/00; applying closure members to bottles, jars or similar containers B67B1/00-B67B6/00; concurrent cleaning, filling and closing of bottles B67C7/00; emptying bottles, jars, cans, casks, barrels or similar containers B67C9/00)
- C07K: PEPTIDES (peptides in foodstuffs A23; obtaining protein compositions for foodstuffs, working-up proteins for foodstuffs A23J; preparations for medicinal purposes A61K; peptides containing beta-lactam rings C07D; cyclic dipeptides not having in their molecule any other peptide link than those which form their ring, e.g. piperazine-2,5-diones, C07D; ergot alkaloids of the cyclic peptide type C07D519/02; macromolecular compounds having statistically distributed amino acid units in their molecules, i.e. when the preparation does not provide for a specific; but for a random sequence of the amino acid units, homopolyamides and block copolyamides derived from amino acids C08G69/00; macromolecular products derived from proteins C08H1/00; preparation of glue or gelatine C09H; single cell proteins, enzymes C12N; genetic engineering processes for obtaining peptides C12N15/00; compositions for measuring or testing processes involving enzymes C12Q; investigation or analysis of biological material G01N33/00)
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)

## Abstract

The enclosed disclosure describes, among other things, a method including the steps of a first deaerating step in which a mixture comprising peptides is deaerated by lowering the pressure, filtering the mixture through a sterilizing filter; and a second deaerating step, in which the filtrate is deaerated by vibration and lowering the pressure.

## Claims

### Claim 1

A method for deaerating and sterilizing a self-assembling peptide solution having at least 0.5 weight % of a self-assembling peptide, the method comprising the steps of:
a first deaerating step wherein the self-assembling peptide solution is deaerated by lowering a pressure on the self-assembling peptide solution to vacuum;
filtering the self-assembling peptide solution through a sterilizing filter thereby producing a self-assembling peptide filtrate; and
a second deaerating step wherein the filtrate is deaerated by vibration at a vibration frequency between 20 and 360 revolutions per minute, and by lowering the pressure on the self-assembling peptide filtrate by at least 0.05 MPa.

### Claim 2 (depends on 1)

The method of claim 1, wherein the sterilizing filter has an average pore size of less than 0.22 μm.

### Claim 3 (depends on 1)

The method of claim 1, wherein the self-assembling peptide comprises one of RADA16-I (SEQ ID NO:1), IEIK13 (SEQ ID NO:39); and KLDL12 (SEQ ID NO:12).

### Claim 4 (depends on 1)

The method of claim 1, wherein the first deaerating step comprises lowering the pressure at a rate of less than 0.01 MPa/min.

### Claim 5 (depends on 1)

The method of claim 1, wherein the first deaerating step occurs in a deaeration chamber and comprises lowering the pressure by at least 0.095 MPa.

### Claim 6 (depends on 5)

The method of claim 5, wherein the pressure is lowered by at least 0.095 MPa for at least 30 minutes.

### Claim 7 (depends on 1)

The method of claim 1, wherein an eccentric distance of the vibration is between −10 cm and 10 cm.

### Claim 8 (depends on 1)

The method of claim 1, wherein the second deaerating step comprises lowering the pressure by at least 0.095 MPa.

### Claim 9 (depends on 1)

The method of claim 1, wherein a step of sterilizing is performed with one of ethylene oxide gas and a hydrogen peroxide gas.

### Claim 10 (depends on 1)

The method of claim 1, wherein the sterilizing filter is constructed from a material selected from the group consisting of the following: cellulose nitrate, cellulose acetate, vinyl polymers, fluorocarbons, polyethylene, ultrahigh molecular weight polyethylene, polypropylene, EVA copolymers and alpha olefins, metallocene olefinic polymers, PFA, MFA, PTFE, polycarbonates, vinyl copolymers, polyamides, nylon, polyesters, cellulose, regenerated cellulose, cellulose composites, polysulfone, polyethersulfone, polyarylsulfone, polyphenylsulfone, polyacrylonitrile, polyvinylidene fluoride (PVDF), and blends thereof.

### Claim 11 (depends on 1)

The method of claim 1, wherein the sterilizing filter is constructed from polyethersulfone.

### Claim 12 (depends on 1)

The method of claim 1, wherein the filtering step comprises a step of filling the sterilizing filter at a first pressure, then increasing the pressure to perform the filtration.

### Claim 13 (depends on 1)

The method of claim 1, wherein the sterilizing filter is washed prior to an integrity test.

### Claim 14 (depends on 13)

The method of claim 13, wherein the sterilizing filter is washed with water prior to the integrity test, and the water is one of above 70° C. and high-pressure of 0.5 MPa or more, or both.

### Claim 15 (depends on 1)

The method of claim 1, wherein the filtering step is performed with two filters operating in parallel.