Transcript SDS-PAGE V4
Methodology for the SDS-PAGE Proteins exhibit different molecular weight depending on the amino acid composition, this property is exploited to separate proteins using SDS-PAGE. The electrophoresis method used to separate proteins based on their molecular weight. Related LOs: Electrophoresis, Amino acid property > Prior Viewing – IDD-11. Protein quantification, IDD-14. Isoelectric focusing, IDD16. Equilibration of IPG strips > Future Viewing – IDD-20. Silver staining, IDD-22. 2D-gel scanning and image Analysis Course Name: SDS-PAGE Level(UG/PG): UG Author(s): Dinesh Raghu, Vinayak Pachapur Mentor: Dr. Sanjeeva Srivastava *The contents in this ppt are licensed under Creative Commons Attribution-NonCommercial-ShareAlike 2.5 India license 1 Learning objectives After interacting with this learning object, the learner will be able to: 1. Define the steps involved in the method 2. Indicate the buffers/reagents used in the method 2 3. 3 4. 4 5. 6. 5 Operate the mechanism of protein separation in SDSPAGE Outline the gradient gels for proper resolution and separation of the proteins. Infer the steps involved to perform Batch processor. Assess the troubleshooting steps involved in the experiments. 1 2 Master Layout Reagent preparation (Slide:5-8) Buffer Preparation (slide:9-11) Cocktail for gel casting (Slide:12-13) 3 Gel casting (Slide:14-19) 4 5 Sample loading and gel running (Slide:20-23) Display a image from each of these steps, with user click. 1 2 Definitions and Keywords 1.Protein: Proteins are the biomolecules, composing of amino acid, which forms the basic building blocks of the system and performs most of the biological function of the system. 2.SDS-PAGE: Sodium dodecyl sulphate –Polyacrylamide Gel Electrophoresis is used for the separation of proteins based the molecular weight of the proteins. The cocktail consists of acrylamide, bisacrylamide, TEMED, SDS, Ammonium persulphate. 3.Acrylamide and bisacrylamide: used as a crosslinker for polymerization reaction to forms the gel like polymer. 3 4. TEMED (Tetramethylethylenediamine): catalysis free radical formation of the ammonium persulphate in the cocktail. 5. Ammonium persulphate : APS helps in the formation of the free radicals that aid in the polymerization reaction of acrylamide and bis acrylamide. 4 6. Stacking gel: has a acidic pH of 6.8 and a low acrylamide concentration of 5.5%. Under these conditions proteins separation is poor but form thin, sharply defined bands at the start of resolving gel 7.Resolving gel: has a basic pH of 8.8, and a higher polyacrylamide of 12.5%. As a protein, concentrated into sharp bands by the stacking gel, travels through the separating gel, the pores have a sieving effect, allowing smaller proteins to separate more faster than higher molecular weight proteins. 5 1 Step 1: T1: Reagent Preparation 2 3 Description of the action 4 5 Show a measuring balance. A hand action when clicked by user should ON the Instrument, pick paper from rack, place it on the balance so that balance reads 0.03g and the user should press ”0” on the balance to make the reading to “0.00”. This action need to be performed for each reagent weighing. Audio Narration (if any) Clean the surface of the balance, Tare the weight of the paper before weighing. 1 2 3 4 5 Step 1: T1: Reagent Preparation Tris-HCL Water 1.5 M Tris-Hcl PH 6.8 1.5 M Tris-Hcl PH 8.8 Description of the action Animator should redraw above figure as shown. Instruct user to weigh Tris-Hcl, user must tare the balance with paper like in slide:5, with help of spatula weigh the required amount (3.15g). Show like the user added excess amount and show user action to remove the excess. Transfer weighed amount to tris-hcl ph 6.8 bottle, followed by addition of water. Animate like the user taking the water and pouring to the 100ml measuring cylinder till the volume reaches 80ml and adding to the bottle (repeat the same weighing and add to bottle labeled as Tris-Hcl ( ph 8.8)). Once water is added let user give a brief spin to dissolve the reagent into the solution. Audio Narration Weigh Tris-Hcl according to experimental design. Give a brief spin to dissolve powder completely. Add half the amount of total volume of water required. Video file: Balancing 1 Step 1: T1: Reagent Preparation 2 NaOH 3 4 5 HCl Description of the action Then the beaker containing(labeled as “tris-hcl pH 6.8”) has to be taken near pH meter and allow the user to dip ph rod in the solution. Animate like the user switching on the pH meter. The meter should show 5.5 in the display and instruct user to add NaOH. Now allow the user to click on NaOH so that drops of NaOH should be added with fillers and the reading should increase like 5.8,5.9.6.1,6.3 and then 6.8(desired pH) and show the making the solution volume to 100ml in measuring cylinder with water. Audio Narration Prepare 6.8 pH tris – Hcl solution 1 Step 1: T1: Reagent Preparation 2 NaOH 3 4 5 HCl Description of the action Follow above steps to prepare Tris-Hcl ph 8.8. To set the pH allow the user to dip ph rod in the solution. Animate like the user switching on the pH meter. The meter should show 5.5 in the display and instruct user to add NaOH. Now allow the user to click on NaOH so that drops of NaOH should be added with fillers and the reading should increase like 5.8,5.9.6.1, 6.3 and then 6.7,6.9,7.4,7.6,7.8,8,8.4,8.6,8.8(desired pH) and show the making the solution volume to 100ml in measuring cylinder with water. Audio Narration Prepare 8.8 pH tris –Hcl solution Video file: pH meter 1 Step 2: T2: Buffer Preparation 2 3 4 5 Description of the action Show a measuring balance. A hand action when clicked by user should ON the Instrument, pick paper from rack, place it on the balance so that balance reads 0.03g and the user should press ”0” on the balance to make the reading to “0.00”. This action need to be performed for each reagent weighing. Audio Narration (if any) Clean the surface of the balance, Tare the weight of the paper before weighing. 1 2 Step 2: T2: SDS running Buffer preparation Tris base SDS Glycine Water 3 4 5 Description of the action Show the bottles labeled as TRIS-Base, Glycine and SDS. The user should click on the required reagent bottle and spatula for weighing. Instruct user to weigh Tris base, let user pick the bottle, uncap it, with help of spatula weigh the 30.3g amount on a paper over the balance. if the gram exceeds user should remove some quantity or if it low add to get required gram. Follow the same instruction for weighing 144.1 g of glycine and 10g SDS and transfer all the content into beaker. Show the measuring cylinder of 1000ml, animate like the user pouring 500ml of water to the cylinder and then to the beaker containing weighed TrisBase,Glycine and SDS. Audio Narration weigh 30.3g of tris base, 144.1g of glycine and 10g SDS accurately. The beaker containing the powder need to be dissolved into the water. 1 Step 2: T2: Buffer preparation 2 Beaker Magnetic bead 3 Description of the action 4 5 Show magnetic stirrer instrument. Let user place the beaker on it. Display the beaker containing powder at bottom, liquid layer on top and a magnetic bead at the bottom. Instruct user to ON the instrument, let user cotrol the speed nob and regulate it accordingly to control the mixing speed in the beaker. Animate powder getting into the solution. Show a turbid solution turning colorless Audio Narration (if any) Prepare 10X SDS running buffer. As an when the powder starts dissolving make up the volume of solution to 1000ml by adding water. Video file: Magnetic stirrer 1 Step 3: T3:Cocktail for gel casting 2 3 4 5 Description of the action Show a measuring balance. A hand action when clicked by user should ON the Instrument, pick paper from rack, place it on the balance so that balance reads 0.03g and the user should press ”0” on the balance to make the reading to “0.00”. This action need to be performed for each reagent weighing. Audio Narration (if any) Clean the surface of the balance, Tare the weight of the paper before weighing. 1 2 Step 3: T3:Cocktail for gel casting SDS APS Water 3 4 Description of the action Show the bottles labeled as APS and SDS.The user should click on the required reagent bottle and spatula for weighing. Instruct user to weigh SDS, let user pick the bottle, uncap it, with help of spatula weigh 0.5g on a paper over the balance. if the gram exceeds user should remove some quantity or if it low add to get required amount. Dissolve the weighed amount by adding 5 ml of water, the user should click on the pipette, set it to 1000ul to take water and add to the weighed SDS (repeat 5 times for 5000ul) and giving a brief mixing on vortex. The same procedure has to be followed for APS preparation. 5 Audio Narration Prepare 10%SDS and 10% APS which are used for the gel casting. 1 Step 4: T4:Gel casting B 2 A 3 Description of the action 4 5 The figure shown above is gel running unit. Please redraw the figure. Instruct user to fix the glass plates, with spacer in-between the plates on either sides using glue and clips. animate all the steps w.r.t figure A. Once plates are ready let user place them in the running unit. The final image B. Audio Narration Clean the glass plates before using.Glass plates need to be fixed in a way there must be no leakage from sides, proper sealing must be done. 1 Step 4: T4: Gel casting Acrylamide mix 2 3 4 5 Tris HCl Gel solution 10% SDS 10% APS TEMED Description of the action Show the bottle labeled as Bisacrylamide and Acrylamide mixture, Tris Hcl (pH8.8) , 10% SDS and 10% Ammonium persulfate, TEMED and water. The user should click on each bottle to measure the required quantity. when the user clicks on Bisacrylamide -Acrylamide, using measuring cylinder user should pour 3ml and 1.5 ml of TrisHcl to the gel solution beaker, animate with pipette action for user adding TEMED, APS and water. (set required volumes on pipette by listening to audio narration) Now give a brief spin to mix the gel solution properly. Audio Narration Prepare 12.5% resolving gel solution consisting of 3 ml acrylamide and bisacrylamide 1.5ml 1.5M Tris –Hcl(pH 8.8),10% 60ul SDS and 10% 60ul APS ,2.11ul TEMED and 1.38ml water. 1 Step 4: T4: Gel casting 2 3 Description of the action Show the running unit, zoom the glass plates which are fixed. Now pour the resolving gel solution into the glass plates. 4 5 ONce Audio Narration Pour the solution at one go, avoid air bubbles. Pour till the solution covers the 75% or 3/4th of the glass plate area. Resolving solution helps for protein separation. 1 Step 4: T4: Gel casting Acrylamide mix 2 3 4 5 Tris HCl Gel solution 10% SDS 10% APS TEMED Description of the action Show the bottle labeled as Bisacrylamide and Acrylamide mixture, Tris Hcl (pH8.8) , 10% SDS and 10% Ammonium persulfate, TEMED and water. The user should click on each bottle to measure the required quantity. when the user clicks on Bisacrylamide -Acrylamide, using measuring cylinder user should pour for 1ml and TrisHcl for 1.8 ml. To the same beaker, animate with pipette action for user adding TEMED, APS and water. (setting the readings as in RHS) Now give a brief spin to mix the solution properly. Audio Narration Prepare stacking gel consisting of 1 ml acrylamide and bisacrylamide 1.8ml 1.5M Tris –Hcl(pH 6.8),10% 75ul SDS and 10% 75ul APS ,4.5ul TEMED and 1.6ml water. . 1 Step 4: T4: Gel casting 2 3 4 5 Description of the action show the running unit, zoom the glass plates which are fixed. Now pour the stacking gel solution into the glass plates. The solution must from a top layer aver the resolving ONcegel. Audio Narration Pour the solution at one go, avoid air bubbles. Pour till the solution covers the top portion of the glass plate area. Stacking gel helps for sample loading. 1 Step 4: T4: Gel casting Comb 2 Image/graphic for the step 3 Description of the action 4 5 once stacking gel solution is poured place a comb on top of the solution. Draw the comb separately as in figure and animate like the user placing the comb on the top of the gel. Place the comb and show like the set up left for 30 minutes Audio Narration Place the comb on the top of the well so that wells are formed for loading the proteins 1 Step 5: T5: Sample loading and gel running Comb 2 Image/graphic for the step 3 4 5 Sample Description of the action After 30m, instruct user to remove the comb. Zoom to show the wells. Let user take out the samples and standard from freezer, place them on ice for thawing for 5min. now let user pipette out the 50ul of standard by taking the pipette and setting to 50ul to add in well 1 and similarly for samples in other wells. After sample and standard loaded, let user fill the running unit with SDS-buffer. Instruct user to cover the running unit and place the electrode and press ON button to start the instrument. Standard Audio Narration Samples in rehydration solution kept in freezer after sample extraction and quantification must be loaded into the wells. Standards acts like a reference marker. And bromophenol blue present in rehydration solution acts like a indicator. 1 Step 5: T5: Sample loading Comb 2 3 4 5 Description of the action Animator should draw a separate Power pack box and draw options like set voltage, time, start and stop buttons. Let user make proper connection of anode and cathode. Animate like the user should click on set to set the voltage to 100V and time 1.30hr and press run. Audio Narration After loading the sample, start the gel run by setting the required voltage and time. 1 Step 5: T5:Sample loading and gel run 2 3 4 5 Description of the action Once the running unit is ON. Animate small air bubbles coming from positive electrode and reaching the top. Also animate that the sample loaded well, blue color band travelling from top to bottom. Re-draw the figure. Audio Narration Mechanism of protein separation: Proteins take up negative charge from SDS present in the buffer, the negatively charged proteins are attracted towards the positive end in the presence of electric field. Proteins start to resolve in gel. Larger protein due to size, move slowly and get separated at the top. while smaller proteins tend to resolve into the gel and start getting separated at the bottom. 1 Step 5: T5:Sample loading and gel run 2 3 4 5 Description of the action Once after the bromophenol blue color band reaches the to positive electrode, instruct user to stop the run. Let user take out the connections, electrode, open the lid, take out the gel. Now the gel plates are ready for scanning or for staining. Audio Narration Soon after the blue band reaches the bottom f the gel, the run must be stopped and gel must be taken for scanning. For more information on gel scanning do follow the future viewing IDD. Slide 58 Tab 01 Slide 911 Tab 02 Slide 12-13 Tab 03 Slide 14-19 Tab 04 Slide 20-23 Tab 05 Tab 06 Tab 07 Name of the section/stage Animation area In Slide-20: let user pour SDS-buffer in little quantity or in-between the run if SDS-buffer level goes low and proceeds with the setup. Instruction: Display on monitor a very low voltage attained with comparison to set voltage on the power pack and instruct user to check the setup again to pour sufficient SDS-buffer till the level making contact with electrode. In Slide-21: if user place the electrode the other way round and proceeds the setup. Interactivity area Button 01 Button 02 Button 03 Instruction: Display on monitor “No voltage, error in setup” and instruct user to check the setup again to place the electrode properly red colored wire in “+” port and black colored wire in “-” port. Instructions/ Working area Credits APPENDIX 1 Questionnaire: Question 1 What is the use of stacking gel? a)To separate proteins b)To increase the resolution c)To separate the contaminants d)To make the sharp bands of protein for better separation in resolving gel Answer: d) To make the sharp bands of protein for better separation in resolving gel Question 2 pH of resolving and stacking gel a)8.8 and 6.8 b)6.8 and 8.8 c)6 and 8 d) Same pH Answer:a) a)8.8 and 6.8 APPENDIX 1 Questionnaire: Question 3 Charge given by the SDS to the protein is a) Negative a)Positive b)No charge c)Neutral Answer: Negative Question 4 Protein moves from a)Negative terminal to positive b)Positive to negative terminal c)Moves based on the charge of the protein d)Doesn’t move Answer: Negative terminal to positive APPENDIX 1 Questionnaire: What is the use of resolving gel? a)To separate proteins based on molecular weight b)To increase the resolution c)To separate the contaminants d)To make the sharp bands of protein for better separation in resolving gel Answer: To separate proteins based on molecular weight APPENDIX 2 Links for further reading Reference websites: 2DE Tutorials by Angelika Görg : http://www.wzw.tum.de/blm/deg/ Books: Biochemistry by Stryer et al., 5th edition Biochemistry by A.L.Lehninger et al., 3rd edition Biochemistry by Voet & Voet, 3rd edition Research papers: Chen JH, Chang YW, Yao CW et al. Plasma proteome of severe acute respiratory syndrome analyzed by two-dimensional gel electrophoresis and mass spectrometry.Proc Natl Acad Sci U S A2004, 7;101(49):17039-44. Eymann C, Dreisbach A, Albrecht D. A comprehensive proteome map of growing Bacillus subtilis cells. Maldonado AM, Echevarría-Zomeño S, Jean-Baptiste S. et al. Evaluation of three different protocols of protein extraction for Arabidopsis thaliana leaf proteome analysis by two-dimensional electrophoresis. Proteomics 2008, 71(4):461-72. APPENDIX 3 Summary The resolving gel and stacking gel composition determine the good separation of protein with high resolution. The molecular weights of the sample proteins can be estimated with the help of co-migrated standards with known molecular weights. The electrophoretic mobility of proteins treated with SDS, depends largely on the molecular weight of the protein. Efficiency of the experiment lies in sample preparation, gel casting with appropriate pH and buffer preparation.