# US 10,478,800 B2 · Highly ordered titania nanotube arrays for phosphoproteomics

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- Number: US 10,478,800 B2
- Document ID: US10478800B2
- Status: Granted
- Kind: B2
- Application number: 15/536,758
- Filed: 2015-12-15
- Published: 2018-01-18
- Granted: 2019-11-19
- Earliest claimed: 2014-12-19
- Assignees: University of Houston System
- Applicants: University of Houston System
- Inventors: Oomman K. Varghese; Aruna Wijeratne; Maggie Paulose; Ivy Ahiabu; Kenneth D. Greis; Dharshana Wijesundara; Wei-Kan Chu
- Web page: https://patentgrep.com/patent/US10478800B2

## CPC

- B01J 20/06: comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J 20/28007: {with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like (carbon nanostructures B01J20/205)}
- B01J 20/28023: {Fibres or filaments (fibres or filaments in the form of membranes B01J20/28038; B01J20/28007 takes precedence)}
- B01J 20/28078: {Pore diameter}
- B01J 20/28083: {being in the range 2-50 nm, i.e. mesopores}
- B01J 20/28085: {being more than 50 nm, i.e. macropores}
- B01J 20/282: Porous sorbents (ion exchange B01J39/00 - B01J41/00)
- B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078}
- C01G 23/047: Titanium dioxide
- C07K 1/145: {by extraction or solubilisation}
- C07K 1/22: Affinity chromatography or related techniques based upon selective absorption processes
- C25D 11/26: of refractory metals or alloys based thereon
- G01N 1/405: {by adsorption or absorption}
- G01N 33/551: the carrier being inorganic
- G01N 33/68: involving proteins, peptides or amino acids {(involving lipoproteins G01N33/92)}
- B01D 15/3828: {Ligand exchange chromatography, e.g. complexation, chelation or metal interaction chromatography}
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/85: by XPS, EDX or EDAX data
- C01P 2004/03: obtained by SEM
- C01P 2004/13: Nanotubes
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- 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)
- C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Titania nanotube arrays are useful for phosphopeptide enrichment and separation. These highly ordered titania nanotube arrays are a low cost and highly effective alternative to the use of liquid chromatography mass spectrometry (LC-MS) methods using meoporous titania beads or particles. The highly ordered TiO2 nanotubes are grown on surfaces coated with Ti metal, or preferably on Ti wires, by methods that preferably include anodic oxidation.

## Claims

### Claim 1

A device for isolation of phosphopeptides in a sample, comprising:
an ordered TiO2 nanotube array comprising ordered TiO2 nanotubes grown on a Ti surface, wherein the nanotubes point outward from the Ti surface, wherein the Ti surface is a Ti wire, and wherein the nanotubes point radially outward from the Ti wire; and
a container for phosphopeptide isolation, wherein the ordered TiO2 nanotube array is located within the container, and wherein the sample is placed in the container to contact the ordered TiO2 nanotube array.

### Claim 2 (depends on 1)

The device of claim 1, wherein the ordered TiO2 nanotubes have a length of about 100 nm to about 500 μm and a pore diameter of about 10 nm to about 400 nm.

### Claim 3 (depends on 1)

The device of claim 1, wherein the ordered TiO2 nanotubes have a length of about 10 to about 20 μm, a pore diameter of about 110 nm, and a wall thickness of about 20 nm.

### Claim 4 (depends on 1)

The device of claim 1, wherein the Ti wire has a diameter of about 0.01 mm to about 1 mm.

### Claim 5 (depends on 1)

The device of claim 1, wherein the Ti wire has a diameter of about 0.25 mm.

### Claim 6 (depends on 1)

The device of claim 1, wherein the ordered TiO2 nanotube array is immobilized on the Ti surface.

### Claim 7 (depends on 1)

A method for isolation of phosphopeptides in a sample, comprising:
exposing a sample containing phosphopeptides to the device of claim 1, wherein the sample is placed in the container and wherein the sample contacts the ordered TiO2 nanotube array to produce bound phosphopeptides attached to the ordered TiO2 nanotube array; and
releasing the bound phosphopeptides from the ordered TiO2 nanotube array to produce isolated phosphopeptides.
