IP Library Granted Patent US 9,725,501
Granted Patent B2
US 9,725,501 · App. 14/294,460 · Granted Aug 8, 2017

Two-stage ultrafiltration/diafiltration

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Quick Facts
Patent No.
US 9,725,501
App. No.
14/294,460
Granted
Aug 8, 2017
Kind
B2
Abstract

The present invention provides a method for concentrating a protein, in particular a method for concentrating a plasma product, in particular IgG, using glycine in a two-stage ultrafiltration/diafiltration approach.

Claims (27)

1. A method for concentrating a plasma product of a solution comprising a protein, the method comprising:

a) ultrafiltering the solution using a first membrane to form a first retentate solution comprising the protein at a first concentration, wherein the first membrane has a molecular weight cutoff sufficient to retain at least a portion of the protein present in the solution;

b) diafiltering the first retentate solution with an aqueous solution using the first membrane to form a second retentate solution comprising the protein at about the first concentration;

c) formulating the second retentate solution comprising the diafiltered protein, with glycine and adjusting the pH to form a formulated second retentate solution; and

d) ultrafiltering the formulated second retentate solution of step c) using a second membrane to form a final retentate solution comprising the protein at a second concentration, wherein the second membrane has a molecular weight cutoff greater than the molecular weight cutoff of the first membrane, wherein the second concentration is greater than the first concentration.

2. The method of claim 1 , wherein the protein is IgG.

3. The method of claim 1 , wherein the first membrane is a polyethersulfone C-screen membrane having a molecular weight cutoff of 50 kDa.

4. The method of claim 1 , wherein the first concentration is about 5% protein (w/v).

5. The method of claim 1 , wherein the second membrane is a hollow fiber membrane or a cassette.

6. The method of claim 1 , wherein the second membrane has a molecular weight cutoff of 100 kDa.

7. The method of claim 1 , wherein the second concentration is at least about 19% protein (w/v).

8. The method of claim 1 , wherein the first membrane has a molecular weight cutoff sufficient to retain at least 90% of the protein present in the solution.

9. The method of claim 4 , wherein, in step c), the about 5% diafiltered protein is formulated to about 0.16 to about 0.30 M glycine and the pH is adjusted to about 4.3.

10. A method for concentrating a protein of a solution comprising the protein, the method comprising:

a) ultrafiltering the solution using a first membrane to form a first retentate solution comprising the protein at a first concentration of about 5%, wherein the first membrane has a molecular weight cutoff sufficient to retain at least about 90% of the protein;

b) diafiltering the first retentate solution using the first membrane with water to form a second retentate solution comprising the protein at about the first concentration;

c) formulating the about 5% diafiltered protein of step b) to about 0.16 to about 0.30 M glycine, wherein the formulating further comprises adjusting pH to about 4.3; and

d) ultrafiltering the second retentate solution using a second membrane to form a final retentate solution comprising the protein at a second concentration of about 19 to about 21%, wherein the second membrane has a molecular weight cutoff greater than the molecular weight cutoff of the first membrane, wherein the second concentration is greater than the first concentration.

11. The method of claim 10 , wherein the protein is IgG.

12. The method of claim 11 , wherein the first membrane has a molecular weight cutoff of about 25 kDa to about 75 kDa.

13. The method of claim 10 , wherein the first membrane has a molecular weight cutoff of about 50 kDa, wherein the second membrane has a molecular weight cutoff of about 100 kDa.

14. The method of claim 10 , wherein the second membrane is a hollow fiber membrane or a cassette.

15. A method for concentrating a plasma product of a solution comprising a protein, the method comprising:

a) ultrafiltering the solution below about 20° C. using a first membrane to form a first retentate solution comprising the protein at a first concentration, wherein the first membrane has a molecular weight cutoff sufficient to retain at least a portion of the protein present in the solution;

b) diafiltering the first retentate solution below about 20° C. with an aqueous solution using the first membrane to form a second retentate solution comprising the protein at about the first concentration;

c) formulating the second retentate solution comprising the diafiltered protein, by adding glycine and adjusting the pH to form a formulated second retentate solution; and

d) ultrafiltering the formulated second retentate solution of step c) below about 20° C. using a second membrane to form a final retentate solution comprising the protein at a second concentration, wherein the second membrane has a molecular weight cutoff greater than the molecular weight cutoff of the first membrane, wherein the second concentration is greater than the first concentration.

Assignments (25)
RELEASE OF SECURITY INTEREST IN PATENTS, RECORDED ON DECEMBER 10, 2021 AT REEL 058480 FRAME 0221 Recorded May 21, 2026
From: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (FORMERLY KNOWN AS GRIFOLS THERAPEUTICS, INC.); GRIFOLS BIOLOGICALS LLC (FORMERLY KNOWN AS GRIFOLS BIOLOGICALS, INC.); BIOMAT USA, INC.; GRIFOLS USA, LLC; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 075614/0936 →
RELEASE OF SECURITY INTEREST Recorded Apr 15, 2026
From: EUROPEAN INVESTMENT BANK
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (F/K/A GRIFOLS THERAPEUTICS, INC.); GRIFOLS BIOLOGICALS LLC (F/K/A GRIFOLS BIOLOGICALS, INC.); BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 075416/0718 →
RELEASE OF SECURITY INTEREST Recorded Apr 15, 2026
From: EUROPEAN INVESTMENT BANK
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (F/K/A GRIFOLS THERAPEUTICS, INC.); GRIFOLS BIOLOGICALS LLC (F/K/A GRIFOLS BIOLOGICALS, INC.); BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 075416/0633 →
RELEASE OF SECURITY INTEREST Recorded Apr 15, 2026
From: THE BANK OF NEW YORK MELLON, LONDON BRANCH
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (F/K/A GRIFOLS THERAPEUTICS, INC.); GRIFOLS BIOLOGICALS LLC (F/K/A GRIFOLS BIOLOGICALS, INC.); GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; BIOMAT USA, INC.; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 075329/0824 →
RELEASE OF SECURITY INTEREST Recorded Apr 15, 2026
From: EUROPEAN INVESTMENT BANK
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (F/K/A GRIFOLS THERAPEUTICS, INC.); GRIFOLS BIOLOGICALS LLC (F/K/A GRIFOLS BIOLOGICALS, INC.); BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 075416/0698 →
SECURITY INTEREST Recorded May 14, 2024
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC; GRIFOLS BIOLOGICALS LLC; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC
To: THE BANK OF NEW YORK MELLON, LONDON BRANCH
Reel/Frame 067409/0127 →
PARTIAL RELEASE OF SECURITY INTEREST Recorded Dec 10, 2021
From: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
To: BIOMAT USA, INC.; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 058480/0221 →
PARTIAL RELEASE OF SECURITY INTEREST IN PATENTS AT REEL/FRAME NO. 51024/0453 Recorded Dec 7, 2021
From: EUROPEAN INVESTMENT BANK
To: BIOMAT USA, INC.; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 058351/0064 →
PARTIAL RELEASE OF SECURITY INTEREST IN PATENTS AT REEL/FRAME NO. 51024/0317 Recorded Dec 7, 2021
From: EUROPEAN INVESTMENT BANK
To: BIOMAT USA, INC.; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 058518/0524 →
PARTIAL RELEASE OF SECURITY INTEREST IN PATENTS AT REEL/FRAME NO. 51021/0593 Recorded Dec 7, 2021
From: EUROPEAN INVESTMENT BANK
To: BIOMAT USA, INC.; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 058350/0980 →
PARTIAL RELEASE OF SECURITY INTEREST IN PATENTS AT REEL/FRAME NO. 51047/0139 Recorded Dec 1, 2021
From: THE BANK OF NEW YORK MELLON, LONDON BRANCH
To: BIOMAT USA, INC.; TALECRIS PLASMA RESOURCES, INC.
Reel/Frame 058292/0564 →
RELEASE OF SECURITY INTEREST Recorded Nov 18, 2019
From: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (FORMERLY KNOWN AS GRIFOLS THERAPEUTICS, INC.); GRIFOLS BIOLOGICALS LLC (FORMERLY KNOWN AS GRIFOLS BIOLOGICALS, INC.); BIOMAT USA, INC.; GRIFOLS DIAGNOSTIC SOLUTIONS INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC
Reel/Frame 051047/0153 →
SECURITY INTEREST Recorded Nov 18, 2019
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC; GRIFOLS BIOLOGICALS LLC; BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
To: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
Reel/Frame 051047/0123 →
SECURITY INTEREST Recorded Nov 18, 2019
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC; GRIFOLS BIOLOGICALS LLC; BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
To: THE BANK OF NEW YORK MELLON, LONDON BRANCH, AS NOTES COLLATERAL AGENT
Reel/Frame 051047/0139 →
RELEASE OF SECURITY INTEREST Recorded Nov 15, 2019
From: EUROPEAN INVESTMENT BANK
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (FORMERLY KNOWN AS GRIFOLS THERAPEUTICS, INC.; GRIFOLS BIOLOGICALS LLC (FORMERLY KNOWN AS GRIFOLS BIOLOGICALS, INC.); BIOMAT USA, INC.; GRIFOLS DIAGNOSTIC SOLUTIONS INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC
Reel/Frame 051064/0021 →
RELEASE OF SECURITY INTEREST Recorded Nov 15, 2019
From: EUROPEAN INVESTMENT BANK
To: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC (FORMERLY KNOWN AS GRIFOLS THERAPEUTICS, INC.); GRIFOLS BIOLOGICALS LLC (FORMERLY KNOWN AS GRIFOLS BIOLOGICALS, INC.); BIOMAT USA, INC.; GRIFOLS DIAGNOSTIC SOLUTIONS INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.
Reel/Frame 051024/0722 →
SECURITY INTEREST Recorded Nov 15, 2019
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC; GRIFOLS BIOLOGICALS LLC; BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
To: EUROPEAN INVESTMENT BANK
Reel/Frame 051024/0453 →
SECURITY INTEREST Recorded Nov 15, 2019
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC; GRIFOLS BIOLOGICALS LLC; BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
To: EUROPEAN INVESTMENT BANK
Reel/Frame 051024/0317 →
SECURITY INTEREST Recorded Nov 15, 2019
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC; GRIFOLS BIOLOGICALS LLC; BIOMAT USA, INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC; TALECRIS PLASMA RESOURCES, INC.
To: EUROPEAN INVESTMENT BANK
Reel/Frame 051021/0593 →
SECURITY INTEREST Recorded Sep 7, 2018
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS LLC; GRIFOLS BIOLOGICALS LLC; BIOMAT USA, INC.; GRIFOLS DIAGNOSTIC SOLUTIONS INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC
To: EUROPEAN INVESTMENT BANK, AS LENDER
Reel/Frame 047438/0836 →
CHANGE OF ADDRESS Recorded Jun 1, 2018
From: GRIFOLS THERAPEUTICS LLC
To: GRIFOLS THERAPEUTICS LLC
Reel/Frame 046286/0824 →
CHANGE OF NAME Recorded Jan 5, 2018
From: GRIFOLS THERAPEUTICS INC.
To: GRIFOLS THERAPEUTICS LLC
Reel/Frame 045008/0573 →
SECURITY INTEREST Recorded Dec 5, 2017
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS INC.; GRIFOLS BIOLOGICALS INC.; BIOMAT USA, INC.; GRIFOLS DIAGNOSTIC SOLUTIONS.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.
To: EUROPEAN INVESTMENT BANK, AS LENDER
Reel/Frame 044696/0846 →
SECURITY INTEREST Recorded Dec 5, 2017
From: GRIFOLS SHARED SERVICES NORTH AMERICA, INC.; GRIFOLS THERAPEUTICS INC.; GRIFOLS BIOLOGICALS INC.; BIOMAT USA, INC.; GRIFOLS DIAGNOSTIC SOLUTIONS.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC
To: EUROPEAN INVESTMENT BANK, AS LENDER
Reel/Frame 044697/0725 →
SECURITY INTEREST Recorded Feb 7, 2017
From: GRIFOLS SHARED SERVICES NORTH AMERICA INC.; GRIFOLS THERAPEUTICS INC.; GRIFOLS BIOLOGICALS INC.; BIOMAT USA, INC.; GRIFOLS DIAGNOSTIC SOLUTIONS INC.; GRIFOLS WORLDWIDE OPERATIONS USA, INC.; GRIFOLS USA, LLC
To: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
Reel/Frame 041651/0487 →