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Detection & Identification Methods

October 24, 2007 MSB B554

Hong Li [email protected] 973-972-8396

Lecture notes: http://njms.umdnj.edu/proweb/lectures/note2007fall01.pdf

Objectives

1. Protein analysis to determine: • Purity, quantity and identity • Expression and localization • Post-translational modification • Induction and turnover 2. Principles behind the analytical techniques • Based on unique physical/chemical properties; size, charge, etc. • Assays are based on reactions producing light, color and radio activities for detection

3. Techniques • Electrophoresis • Immunoblotting • Autoradiography •

1 Purity, quantity and identity

Post-translational modification Induction and turnover

Expression localization

Basic Principles for Analysis (How to differentiate one protein from another?)

„ Structure (Drs. Wang & Wah) ‰ composition ‰ Post-translational modification (Dr. Wagner) ‰ Size ‰ Polarity/Charge/Hydrophobicity ‰ Shape ‰ Affinity (binding to other /molecules)

„ Function: catalytic activities

2 Shapes and sizes # of amino acids, composition & sequences

Charges and polarity

3 Charges and polarity from post-translational modifications

Reactivities of amino acids

„ Physical/chemical reactions to facilitate colorimetric detection „ Example: Protein concentration assays: Bradford, BCA, Lowry & Biuret, etc. http://www-class.unl.edu/biochem/protein_assay/

4 Bradford (Bio-Rad)

„ Based on a dye binding to basic and aromatic amino acids „ Coommassie Brilliant Blue (CBB) G250 „ Protein binding causes its maximum absorbance to shift from 465 nm to 595 nm (blue)

Bradford assay

5 Techniques

„ Electrophoresis: separation by size

‰ SDS-PAGE „ Isoelectric focusing: separation by charge „ 2-Dimensional „ Immunoblotting: detection by specific affinity with antibodies (a special class of proteins) „ Autoradiography: radioactivity „ Mass spectrometry: protein /identification „ Proteomics: high-throughput analysis

Electrophoresis

„ Physics: Charged particles in an electric field will migrate according to their charge-to-mass (size) ratio „ Positively-charged molecules migrates towards anode (negative pole) while negatively-charged molecules migrates toward cathode (positive pole) „ Electrophoresis medium creates frictions during the migration. Protein shape has an impact: globular proteins migrate faster while cylindrical proteins migrate slower.

6 Sodium Dodecylsulfate polyacrylamide gel electrophoresis (SDS-PAGE)

A method for protein separation and visualization based on size

Acrylamide polymerization & effect on protein separation

www.nationaldiagnostics.com www.cas.vanderbilt.edu/bsci111a/protein-electro/supplemental.htm

7 SDS: Protein Denaturation Protein denaturation

PAGE

SDS: minimize the impacts of protein charge and shape

Results: Separation by size!

8 Visualization

1. CBB 2. Silver 3. Fluorescent dyes

More….

Example: determine purity

9 Protein size estimation

Human Proteins Size Distribution

10 Additional visualization methods

„ Immunoblotting: a method for specific detection of a protein „ based on the specific binding between protein of interest and a member of a class of proteins, called antibodies „ AKA: Western Blotting

11 Immunoblotting for specific

Using radioisotopes to label and detect proteins

32P-ATP can be used metabolically to label phosphoproteins

35S-Met can be used to label almost all proteins

12 Isoelectric focusing (IEF)

„ A special type of electrophoresis for protein separation: based on charge „ (pI): the pH value at which a protein carries no net charge. (http://www.biology-online.org/dictionary/Isoelectric_point) „ pH < pI: net + charge „ pH > pI: net – charge „ IEF matrix: a gel strip containing an immoblized pH gradient, charged proteins migrate to either cathode and anode crossing different pH steps „ When migrate to their pI, protein will carry no net charge, therefore, no more mobility in an IEF device

Isoelectric point (pI)

pI=(2.1+3.9)/2=3.0

13 Question: How will selected PTM affects protein pI?

2-Dimensional gel electrophoresis (2DE)

14 2DE

2DE Example

An effective tool for proteomics studies.

15 Proteomics

„ Simplified definition: systematic studies of protein structural and functional changes „ 2DE: a tool for protein expression comparison between 2 systems „ Mass spectrometry: a method that uses an instrument, called mass spectrometer to determine the precise mass (size) and the sequence of proteins.

Changes in protein expression is important for cell function

16 2DE Protein Expression Analysis in Proteomics

A B

Excise spot; elute; digest Extract ; MS analyze Protein identification

Each amino acid has an unique mass

17 Mass Spectrometer (MS) for Protein Identification

Sample Preparation Cut spots

Gel Electrophoresis

tryptic digestion cleaves protein at R and K residues Ions

2. Peptide sequencing by MS/MS

1. MS Analysis

PMF spectrum

MS/MS Spectra

Ions vs. Molecules

18 MS analysis of peptides: separation based on mass/charge (m/z) ratio

Mass Spectrometer

19 Peptide Mass Mapping

Mass Spectrometer (MS) for Protein Identification

Sample Preparation Cut spots

Gel Electrophoresis

tryptic digestion cleaves protein at R and K residues Peptide Ions

Peptide sequencing by MS

MS Analysis

PMF spectrum

MS/MS Spectra

20 Mass Spectrometry – MS Measuring peptide mass

MS spectrum

21 : peptide sequence determination

Peptide sequencing by MS

MS Analysis

PMF spectrum

MS/MS Spectra

MS is able to “fragment” a peptide into many smaller peptide ions

22 Mass difference between fragments can be used for peptide sequencing

G V Y 57 99 163

Amino acid properties

23 Question: How will selected PTM affects amino acid mass?

+80 Da to ser

Q: Protein

If these two spots are the same protein but differ by phosphorylation, which one may be phosphorylated?

A B

24 Example: Identification of Proteins in cellular organelles

25 Protein detection and identification methods

1. SDS-PAGE: protein separation based on size 2. IEF: protein separation based on pI 3. 2DE: protein separation based on pI and size 4. Coommassie Brilliant Blue: a dye for protein concentration assay and general detection in gel electrophoresis 5. Immunoblotting: a sensitive and specific method for detecting interested proteins separated by gel electrophoresis 6. Autoradiography: a sensitive and highly quantitative method for studying dynamic changes of proteins separated by gel electrophoresis 7. Mass spectrometry: a method for and identification 8. Proteomics: systematic studies of protein structural and functional changes using all the tools described above

26 For more information: Take advanced classes!

„ Introduction to genomics, proteomics and „ Advanced genomics, proteomics and bioinformatics „ Protein course „ Analytical methods

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