Team:UNSW Australia/Notebook


Team: UNSW Australia


Notebook

Overview

All of our lab work were documented using Benchling. We've separated our lab work into cloning work and proteins expression & purification. Click on the buttons on the right side to toggle the lab notes for the respective categories.

Week 1

15 April - 21 April

Protein Expression & Purification

  • Overnight culture of alpha and beta prefoldins with catcher.
  • Expression of prefoldins by IPTG induction in T7 express cells.
  • Bug buster and SDS-PAGE gel run to check for protein size.
  • Gel showed beta prefoldin as a strong band at the correct size however alpha was too small and possibly did not contain the fused catcher protein.

Week 2

22 April - 28 April

Protein Expression & Purification

  • Overnight culture of alpha and beta prefoldins with catcher.
  • Expression of prefoldins by IPTG induction in T7 express cells.
  • Freezing of samples

Week 8

3 June - 9 June

Cloning

  • PC2 lab induction.
  • Construct lab plan, compile protocols and reagent list.

Protein Expression & Purification

  • Lab induction
  • Lab plan written
  • Ordered materials

Week 9

10 June - 16 June

Cloning

  • Design and order G-blocks for DBAT, Duke's DBAT, LXYL-P1-2, TycA and PAM enzymes from IDT.

Protein Expression & Purification

  • Meeting with supervisor to discuss lab plan

Week 10

17 June - 23 June

Cloning

  • Preparation of Luria Broth Agar with Ampicillin plates.
  • Small scale grow up of pET19b plasmid containing competent Dh5-alpha E.coli cells.
  • pET19b plasmid extracted and purified using Promega miniprep kit, plasmid concentration and purity quantified by nanodrop.

Protein Expression & Purification

  • Building induction/ OGTR Induction.

Week 11

24 June - 30 June

DNA

  • Calculate PCR thermocycling conditions and mastermix contents.

Protein Expression & Purification

  • Bug-buster and SDS-PAGE of samples prepared in week 2 (α-PFD + Catcher before and after IPTG induction, β-PFD + Catcher before and after IPTG induction).
  • SDS-PAGE gels showed expression of all proteins was achieved in the soluble fraction however there was a low expression of alpha prefoldin, and beta-prefoldin was found in the insoluble fraction.
  • Following successful expression results, cells were lysed via sonication by Nga, spun down and separated into soluble and insoluble fractions of proteins.
  • Soluble and insoluble protein was prepared and incubated onto Ni-NTA beads (soluble α+β, insoluble α, insoluble β) then loaded onto gravity columns for elution by buffers with different imidazole concentrations into fractions.
  • Elution fractions were run on SDS-PAGE to show presence of more pure protein.
  • Made buffers for Ni-NTA Histrap protein purification (binding and elution buffers) and insoluble fraction denaturing (triton 1X and guanidine denaturing buffer).
  • Made PC2 labels for chemicals.

Week 12

1 July - 7 July

Cloning

  • Linearise pET19b backbone by PCR amplification (Phusion DNA polymerase). The concentration and purity quantified by nanodrop, then visualised by agarose gel electrophorepsis.
  • Rerun PCR of pET19b backbone with optimised annealing temperature.
  • Circular plasmid DNA removed by DpnI digest (NEB), purified using QIAGEN PCR clean up kit.
  • Gibson assembly of G-blocks into pET19b backbone, concentration and purity of DNA quanitified by nanodrop.
  • Transformation of assembled constructs into competent T7 Express E.coli (NEB), then plated onto selection plates with Ampicillin and grown overnight.

Protein Expression & Purification

  • Prepare Bolt MES buffer and protein fixative buffer (25% isopropanol, 10% acetic acid) for PAGE gels
  • .
  • Prepared elution buffer concentration gradient solutions for His-tag protein purification.
  • Starter culture of prefoldins (α-PFD, α-PFD + Catcher, β-PFD, β-PFD + Catcher) in 10ml Luria broth overnight with ampicillin.
  • Addition of starter cultures into separate autoclaved LB broths (1 L) with ampicillin at 1 X concentration with incubation at 37°C, 200 rpm (for fast growing) until 0.6 OD is reached.
  • Cultures were induced with IPTG and incubated at 20°C, 200 rpm overnight (for protein production).
  • Bug buster of induced and non-induced (control) samples of alpha, alpha +C, beta, beta +C, followed by SDS-PAGE to show protein production in response to IPTG induction and presence of proteins in soluble fractions (apart from beta and beta plus catcher which appeared in the insoluble fraction).
  • Spin down culture to form pellets and freeze in -40°C.
  • Filter and degas solvents to be used for AKTA in week 13.
  • Training for AKTA start (chromatography machine for protein purification) and sonicator (for cell lysis).

WEEK 13

8 July - 14 July

Cloning

  • Gibson assembly of TycA into pET19b, troubleshooting molar ratio, transformed into T7 Express E.coli and grown overnight.
  • Small scale grow up of DBAT, Duke's DBAT, PAM, LYXL and TycA.
  • Extraction and purification of plasmids by miniprep (QIAGEN), quantified by nanodrop.

Protein Expression & Purification

  • Cell lysis by sonication of pellet samples prepared in week 12
  • Purify alpha +C, beta +C and alpha via AKTA start machine
  • SDS-PAGE of fractions which showed clean proteins for all samples without contaminants however lots of protein was found in flow though (did not originally bind well to column)
  • Concentration and buffer exchange of alpha +C, beta + C and alpha however beta + C precipitated in the concentration tube (may need to use dialysis for buffer exchange instead)
  • BCA assay on beta +C, alpha w/ and without catcher to determine protein concentrations
  • Reload alpha +C and beta +C flow-through on AKTA to collect protein found in original flow-through
  • SDS page found flow through of second AKTA run still contained a lot of his-tagged protein not bound to column.

Week 14

15 July - 21 July

Cloning

  • Plasmid DNA concentrated using Promega DNA clean up Kit.
  • Small scale grow up, miniprep (QIAGEN) of TycA, PAM, Duke's DBAT and LXYL containing E.coli strains.
  • Samples submitted for sequencing by Ramaciotti Centre for Genomics.

Week 15

22 July - 28 July

Cloning

  • Replated DBAT, PAM, TycA and LXYL strains.
  • Ordered S. cerevisiae codon optimised LXYL-P1-2 gBlock from IDT.
  • Compiled reagent list and protocols for transformation of LXYL-P1-2 into S. cerevisiae.
  • Preparation of YEPD media and agar plates.
  • Obtained S. cerevisiae BY4741 strain, courtesy of Marc Wilkin's Laboratory.

Protein Expression & Purification

  • Run alpha flow-through on AKTA to collect protein found in original flow-through.
  • Lyse E.coli cells containing beta prefoldin (from week 12 pellet samples) via sonication, and incubate washed Ni-NTA resin with supernatant (soluble protein).
  • Wash resin and elute beta prefoldin from gravity column.
  • SDS-PAGE, found beta prefoldin protein in fractions with limited contamination from other proteins.
  • Concentration of alpha +C, alpha, beta +C and beta samples and flow-throughs.
  • BCA assay for all four prefoldins to determine protein concentrations.

Week 16

29 July - 4 August

Cloning

  • Colony PCR of DBAT, LXYL, TycA, PAM and Duke's DBAT, amplified sequences visualised by gel electrophoresis.
  • Designed primers to add "TAA" stop codon by PCR-directed codon addition of Duke's DBAT, primers ordered from Sigma Aldrich.

Week 18

12 August - 18 August

Cloning

  • PCR-directed codon addition of Duke's DBAT, visualisation of PCR product by gel electrophoresis and quantified by nanodrop.
  • PCR-directed codon addition repeated with changes to annealing temperature and extension time.
  • Ligation of LXYL S. cerevisiae pD1204 construct by Golden gate assembly and transformed into T7 Express E.coli.
  • Gibson Assembly of Duke's DBAT, TycA, and LXYL into pET19b, pET19b and LXYL+pD1204 constructs transformed into T7 Express E. coli.
  • The following was performed on the transformants: Small scale grow up, plasmid DNA extracted (QIAGEN miniprep kit), submitted for sequencing (Ramaciotti Centre for Genomics), colony PCR, gel electrophoresis and glycerol stocks for long term storage.

Protein Expression & Purification

  • Starter cultures of alpha and beta prefoldins with and without catcher.
  • Large scale grow-up and IPTG induction.
  • Bug buster and SDS-PAGE found all samples contained protein but their was slightly less beta prefoldin protein than others.
  • Pellets were harvested and stored in the -40°C freezer.

Week 19

19 August - 25 August

Cloning

  • Sequence alignment of constructs, unsuccessful assembly.
  • Ordered Duke's DBAT gBlock with stop codon from IDT.

Week 20

26 August - 1 September

Cloning

  • Gibson assembly of Duke's DBAT and pET19b, construct transformed into T7 Express E. coli.
  • DBAT, PAM, LXYL(e) and TycA plasmids submitted for sequencing. Insert amplified by PCR and visualised by gel electrophoresis.
  • Colony PCR of LXYL(s), visualised by gel electrophoresis.
  • Small scale grow up, miniprep and glycerol stocks of Duke's DBAT, LXYL(e), LXYL(s) and TycA.
  • Research on possible assays for characterisation ATF1.

Protein Expression & Purification

  • Purification of alpha +C, beta +C and alpha using AKTA start machine.
  • Concentration of alpha +C, alpha, beta +C and beta samples and flow-throughs.
  • Starter cultures of beta, PAM and DBAT prepared.
  • Large scale grow-up and IPTG induction.
  • PAM and DBAT pellets were harvested and stored in -40°C freezer.

Week 21

2 September - 8 September

Cloning

  • Colony PCR of LXYL(e), Duke's DBAT and TycA under optimal annealing temperatures and extension times
  • Golden gate assembly of LXYL-P1-2 into pD1204 (provided by Joshua Hamey) and transformation into T7 Express E. coli
  • Grow up of U, T, L(e), L(y), miniprep and samples submission for sequencing (Ramaciotti Centre)
  • Gibson assembly of TycA+pET19b with time, concentration and gibson master mix controls. Transformed into T7 Express E. coli
  • LXYL(e) gibson assembly and transformation
  • Grow up of TycA and Duke DBAT and miniprep
  • Prepared LB Agar and Chloramphenicol plates
  • Transformed linear pSB1C3 and RFP+pSB1C3 into competent HB101 E.coli and plated
  • Restreaked pink colonies on new plates to test plate batches

Protein Expression & Purification

  • BCA assay for all four prefoldins to determine protein concentrations.
  • Bug buster of PAM and DBAT showed good beta expression. However, lots of PAM in the insoluble fraction and no DBAT expression could be seen.
  • Native page was performed on prefoldins to demonstrate assembly of assemblase hexameric scaffold. Successful results of assembly were achieved.
  • Gravity column purification of PAM and DBAT yielded no soluble protein thus purification was unsuccessful.
  • Purification of beta via AKTA start machine.

Week 22

9 September - 15 September

Cloning

  • Sequence alignment.
  • Submit TycA#3 and Duke#1 for sequencing (Ramaciotti).
  • LXYL(e) gibson assembly and transformation.
  • Resuspended and transformed ATF1 (alcohol acetyltransferase) into HB101 E.coli, plated and grown overnight.
  • Remade LB Agar + CAM plates.
  • Troubleshoot Agar plates with RFP and linear controls and transformed into T7 Express E. coli.
  • Troubleshoot CAM plates with known CAM resistant strains.
  • Resuspended Red Luciferase and EPIC Luciferase DNA and transformed into T7 Express E.coli.
  • Grow up of ATF, Red Luciferase and EPIC Luciferase.
  • Colony PCR and miniprep of ATF, Red Luciferase and EPIC Luciferase. Visualised by gel electrophoresis.

Protein Expression & Purification

  • Expression conditions were tested (IPTG and temperature) for PAM and DBAT.
  • Bug buster of the different PAM and DBAT cultures were still insoluble.
  • Purification by AKTA for PAM and DBAT samples show no protein binding and elution from the column.
  • The Ellman’s assay was tested and a standard curve as constructed.

Week 23

16 September - 22 September

Cloning

  • Gel of TycA, Duke’s DBAT, LXYL+pET19b and LXYL+pD1204.
  • Restriction enzyme digest of TycA, Duke’s DBAT, LXYL+pET19b, DBAT, PAM. Visualised by gel electrophoresis.
  • Colony PCR of ATF colonies, imaged by gel electrophoresis.
  • DpnI digest and PCR clean up of ATF4, ATF28 and ATF29 PCR products.
  • Gibson assembly of ATF4, ATF28, ATF29 colonies and transformation into T7 Express cells.
  • Colony PCR of ATF28/29, visualised by gel electrophoresis.
  • Concentrate PAM and DBAT fractions and run on gel.

Protein Expression & Purification

  • A 1L expression of alpha +C and beta +C was performed.
  • More expression conditions for PAM and DBAT were tested.
  • Bug buster shows expression of insoluble PAM while DBAT cultures contain both soluble and insoluble protein.
  • SDS-PAGE of cell free lysate and soluble fraction of cultures reconfirms findings.
  • Purification of alpha+C and beta+C as well as one PAM and one DBAT sample on AKTA.
  • Buffer exchange of alpha+C and beta+C via dialysis.
  • Concentration of PAM and DBAT fractions were run on gel showing very light PAM and DBAT bands.

Week 24

23 September - 29 September

cloning

  • Colony PCR of mCerulean3, TycA and ATF1 #28.
  • DpnI digest (NEB) and DNA clean up (QIAGEN) of mCerulean3 and ATF1 fragments.
  • Gibson assembly of mCerulean3, TycA, LXYL, Duke's DBAT and ATF1 into pET19b and transformed into T7 Express E.coli.
  • Colony PCR of mCerulean3, TycA, LXYL, Duke's DBAT and ATF1. DNA fragments visualised by gel electrophoresis on a 1% agarose gel.
  • Small scale grow up and miniprep of positive colonies.

Protein Expression & Purification

  • Purified and non-purified PAM and DBAT bands were excised from SDS-PAGE gel and sent for mass spectrometry analysis. Results show both PAM and DBAT are present in the soluble fractions however PAM is at a very low concnetration.
  • Expression of 1 L PAM cultures (0mM IPTG and 0.1 mM IPTG).
  • Bug buster performed on PAM cultures. Both showed PAM in insoluble fraction.
  • PAM (0.1 mM IPTG) was purified again on akta and fractions were concentrated and run on SDS PAGE gel
  • Conjugation between PAM-Snooptag and beta prefoldin- SnoopCatcher was tested yielding negative results.
  • Conjugation between alpha PFD and beta PFD on Native PAGE gel shows good results but need adjustments of protein ratios.

Week 25

30 September - 6 October

Cloning

  • Submitted Duke's DBAT, mCerulean3, ATF1 and TycA for sequencing (Ramaciotti Centre).
  • Restriction enzyme digest of plasmid DNA. Visualised by gel electrophoresis.
  • Sequence alignment check.
  • Colony PCR of TycA. Amplicon visualised by gel electrophoresis.
  • Preparation of 1000X Ampicillin stocks.
  • Small scale grow up of PAM, TycA and gamma-prefoldin DNA. Plasmid DNA extracted and purified by miniprep (QIAGEN). DNA concentration and purity quanitified by nanodrop.
  • Transformation of PAM into Origami 2(DE3)pLysS Competent Cells.

Protein Expression & Purification

  • Purification of ATF1 for biobrick characterisation was performed.
  • Assays on ATF1 activity were unsucessful.
  • TycA, DUKE, ATF1 and mCerulean colonies were grown up, expressed and purified with DUKE, ATF1 and mCerulean showing expressed protein determined by bug buster.
  • Grow up of alpha PFD beta PFD, PAM, DBAT and ATF1 was performed to keep pellets for later use.
  • Beta and alpha PFD was purified on AKTA start machine.
  • BCA assay on alpha PFD, beta PFD, mCerulean3 and mVenus gave approximate concentrations of proteins.
  • Grow up of alpha PFD beta PFD, PAM, DBAT and ATF1 was performed to keep pellets for later use.
  • Native Page was performed on alpha and beta PFD, yielding good results.
  • Conjugation between alpha PFD and venus and beta PFD and cerulean yielded good conjugation.
  • Concentration and buffer exchange of +c, b+b, mCerulean and Venus.
  • Grew up alpha and beta and purified beta.
  • .
  • BCA assay was performed on a+c, b+b, mCerulean and Venus to determine protein concentration.
  • Ellman assay of ATF1 was performed however was unsucessful
  • SDS-PAGE gel of mCerulean3-SnoopTag with BPFD-SnoopCatcher and mCerulean3 (no tag) with BPFD-SnoopCatcher was run to show catcher-tag conjugation however one sample was incomplete.

Week 26

7 October - 13 October

Protein Expression & Purification

  • FRET was attempted twice however was unsuccessful.
  • Native Page was performed on new alpha and beta PFD protein stocks yielding good results.
  • Ellman assay of DBAT was performed however was unsucessful.
  • Large scale grow up, espression and purification of PAM was performed.
  • SDS-PAGE gel of mCerulean3-SnoopTag with BPFD-SnoopCatcher and mCerulean3 (no tag) with BPFD-SnoopCatcher was run to show catcher-tag conjugation yielding good results.
  • Bug buster of DUKE, DBAT and PAM was performed.
  • ATF1 was expressed, purified, concentrated, buffer exchnaged and run on BCA assay to determine protein concentration.
  • Grow up and expression of PAM in Origami strain was performed twice however appeared to yeild no protein determined by bug buster.
  • NMR spectra of alpha and beta-phenylalanine were taken as proof of concept for using NMR for PAM enzymatic assay.

Week 27

14 October - 20 October

Protein Expression & Purification

  • Expresseion and purification of DBAT using 6M urea on gravity column.
  • Conjugation of DBAT-SnoopTag with BPFD-SnoopCatcher and PAM-SpyTag with aPFD-SpyCatcher using different concentration of Urea was unsucessful.
  • SDS-PAGE gel of mCerulean3-SnoopTag with BPFD-SnoopCatcher and mCerulean3 (no tag) with BPFD-SnoopCatcher was run to show catcher-tag conjugation.
  • Expression, purification, buffer exchange and concentration of ATF1 was performed.
  • Expression and purification, of DBAT was performed.
  • NMR spectra of deacetyl-paclitaxel was taken as proof of concept for using NMR for DBAT enzymatic assay.