Analytical method for determining the concentration of oxidized nanofibrillar cellulose in a sample

Patent metadata

Field	Value
Publication number	US-10520485-B2
Application number	US-201414783735-A
Country	US
Kind code	B2
Filing date	Apr 11, 2014
Priority date	Apr 12, 2013
Publication date	Dec 31, 2019
Grant date	Dec 31, 2019

Abstract

The present invention provides a method for determining carbonyl ratio and/or concentration of oxidized nanofibrillar cellulose in a sample. In accordance with the invention oxidized nanofibrillar cellulose comprised in the sample is enzymatically hydrolyzed into oxidized cellobioses which are specific markers to oxidized nanofibrillar cellulose. The cellobioses may be then analyzed and quantified to reveal the amount of oxidized nanofibrillar cellulose in the sample. A method for determining the concentration of oxidized nanofibrillar cellulose in a sample comprises steps of providing an analytical sample of material comprising oxidized nanofibrillar cellulose; hydrolyzing the analytical sample to breakdown products of oxidized nanofibrillar cellulose in presence of one or more enzymes; subjecting the breakdown products to a separation analysis to reveal the relative amounts of the breakdown products; and determining the concentration of oxidized nanofibrillar cellu-lose.

First claim

The invention claimed is:

1. A method for determining the concentration of oxidized nanofibrillar cellulose in an analytical sample, the method comprising:
(a) providing an analytical sample of material comprising oxidized nanofibrillar cellulose;
(b) hydrolyzing the analytical sample to breakdown products of the oxidized nanofibrillar cellulose in the presence of one or more enzymes, the breakdown products comprising monosaccharides and oxidized cellobiose;
(c) subjecting the breakdown products to a separation analysis including analytical chromatography to separate the oxidized cellobiose and the monosaccharides to reveal the relative amounts of the breakdown products; and
(d) determining the concentration of the oxidized nanofibrillar cellulose, wherein the concentration of the oxidized nanofibrillar cellulose is determined by comparing the relative amounts of the oxidized cellobiose in the analytical sample to at least two samples comprising different predetermined amounts of oxidized nanofibrillar cellulose.

2. The method as claimed in claim 1 , wherein oxidized cellobiose is GlcA(b1-4)Glc, Glc(b1-4)GlcA, Glc(C6-aldehyde)(b1-4)Glc, and/or Glc(b1-4)Glc(C6-aldehyde).

3. The method as claimed in claim 1 , wherein step (a) further comprises treating the material comprising oxidized nanofibrillar cellulose to obtain a homogenous analytical sample of the material comprising oxidized nanofibrillar cellulose, the treating including cutting, tearing, mixing, grinding, ball milling, sonication, refining, suspending in water, or any combination thereof.

4. The method as claimed in claim 1 , wherein the one or more enzymes in step (b) are selected from the group consisting of cellulases and hemicellulases.

5. The method as claimed in claim 4 , wherein the one or more enzymes in step (b) are selected from the group consisting of endoglucanases, cellobiohydrolases, xylanases, mannanases, β-D-glycosidases, β-D-xylosidases and β-D-mannosidases.

6. The method as claimed in claim 4 , wherein the one or more enzymes of step (b) further comprises pectinases.

7. The method as claimed in claim 1 , wherein the hydrolysis is carried out at a temperature ranging from 15 to 75° C.

8. The method as claimed in claim 1 , wherein step (d) comprises determining an aldehyde and carboxylic acid ratio of the oxidized nanofibrillar cellulose.

9. The method as claimed in claim 8 , wherein the aldehyde and carboxylic acid ratio is determined by comparing the relative amounts of GlcA(b1-4)Glc, Glc(b1-4)GlcA, Glc(C6-aldehyde)(b1-4)Glc, and/or Glc(b1-4)Glc(C6-aldehyde).

10. The method as claimed in claim 1 , wherein in step (c) the separation analysis is analytical chromatography.

11. The method as claimed in claim 10 , wherein analytical chromatography is high-performance liquid chromatography (HPLC) or high-performance anion exchange chromatography (HPAEC) coupled with a mass detector and/or pulsed amperometry detector (PAD).

12. The method as claimed in claim 10 , wherein separation analysis is performed with HPAEC-PAD and a single quadrupole mass spectrometer (MSQ).

13. The method as claimed in claim 1 , wherein the material comprising oxidized nanofibrillar cellulose is selected from the group consisting of paper, cardboard, pulp, pulping liquor, and cellulose based nonwovens.

14. The method as claimed in claim 1 , wherein the material comprising oxidized nanofibrillar cellulose is an aqueous solution.

15. The method of claim 1 , wherein the hydrolysis is carried out at a temperature ranging from room temperature to about 50° C.

16. The method of claim 1 , wherein the hydrolysis is carried out at a temperature ranging from about 35° C. to about 45° C.

Assignees

• Upm Kymmene Corp

Inventors

• Laukkanen Antti
• Pere Jaakko
• Mikkelson Atte

Classifications

• G01N2333/94

  acting on alpha-galactose-glycoside bonds, e.g. alpha-galactosidase · CPC title

• C12Y302/01022

  Alpha-galactosidase (3.2.1.22) · CPC title

• G01N33/34 Primary

  Paper · CPC title

• C12Y302/01025

  Beta-mannosidase (3.2.1.25), i.e. mannanase · CPC title

• C12Q1/40

  involving amylase · CPC title