Showing posts with label TLC. Show all posts
Showing posts with label TLC. Show all posts

Friday, 13 July 2018

DAY 676

Jul 9

1) Today was a rather tiring day, and it was all due to one particular experiment. I spent literally the whole day (from around 8.30am till 9pm) doing one part of this really, really tedious experiment. It's basically silica gel column chromatography (which is meant to purify compounds) turned up to 11. We had a lot of compound to be purified, so obviously, the experiment took much longer.

2) All through the afternoon and evening I was preoccupied with ensuring all the product (collected in those conical flasks you can see below) had been collected. This involved doing a thin-layer chromatography (TLC) after all five conical flasks had been filled. The problem was there was a lot of product to be removed, and even more solution to begin with! So I ended up with the following cycle - prepare solvent, add solvent to column, pump solution out into conical flask, collect into all five conical flasks, do TLC, rinse and repeat ad nauseam.

3) After what I can only assume is a very long time, Chris said not to bother with the rest of the product. On the TLC, the spot (for the product) was getting fainter and fainter - indicating that there was much less product than before. However, the spot was always there (if it was absent that would indicate that we had finished retrieving all our product that we wanted). So we ignored that last bit of product, and focused on evaporating our collected solution.

4) By around 8pm, we had finished evaporating and vacuuming our compound (evaporation to remove the solvent and vacuum to remove any excess moisture). All that was left to do was test this compound to make sure we had synthesised it correctly. Time for mass spectrometry then. Ran the compound over 10 minutes and found the single solitary peak we wanted - that was perfect!

5) Given that this was just one intermediate in a sea of intermediates leading to the final product, I think we can all appreciate the role of a scientist/ researcher in synthesising and optimising complex compounds from scratch. Anyway, that has been my long (and tiring!) day, and I hope you enjoyed reading about it. Thanks very much for visiting, and have a nice weekend ahead. Cheers! :)

Silica gel column chromatography

Lunch with friends
Huge fried chicken thigh, potato strips, and "mapo" tofu (麻婆豆腐)
"Mapo" tofu is tofu (beancurd) set in a spicy sauce, typically a thin, oily, and bright red suspension, based on douban 豆瓣 (fermented broadbean and chili paste) and douchi 豆豉 (fermented black beans), along with minced meat

Thin layer chromatography on a much larger scale...

Had my first taste of "jiaozi" (饺子) in China
(Jiaozi is a kind of Chinese dumpling consisting of a filling of ground meat and/or vegetable filling wrapped into a thinly rolled piece of dough, which is then sealed by pressing the two sides together. 

The "jiaozi" that I had is called "xiang gu ji rou jiaozi" (香菇鸡肉饺子) or "shiitake mushroom and chicken dumplings". Tasted absolutely wonderful! :D

A nitrogen gas leak caused this valve to freeze over - oh look what happens if a random finger pokes it...

A trail of water results as the leak cannot repaired - the ice almost instantly vaporises!

Tuesday, 25 July 2017

DAY 326/327

Jul 24 & 25

1) All good things must come to an end, so the saying goes. And just like that, my summer research is drawing to a close. It has been an absolute privilege working at the Apjohn Chemistry Research Laboratory, under my Principal Investigator, Dr. Darren Griffith.

2) Less than two months ago, I started work here as a summer research student, under the RCSI Research Summer School programme. My project was entitled, "Novel Bismuth Compounds as Potential Antimicrobial Drugs". We wanted to combine the antimicrobial properties of bismuth with the Fe-binding properties of iron chelators.

3) And here to help me throughout that journey was Mr. Donal Keogan, a final year PhD student. Under their superb tutelage and guidance, my love for chemistry and research as a whole grew. I've a newfound appreciation for the researchers working long shifts in the labs; uncertain if their reactions would turn out successful or not.

4) Most of the time, my day would begin at around 9.00am, where I'd set up an experiment. Sometimes analysis of a product was required, so we'd head over to York House to do mass spectrometry or NMR spectroscopy. Other analytical methods such as X-ray crystallography and elemental analysis had to be sent off to various labs for testing, as we didn't have the required facilities.

5) I'll cherish the growth and progress that I've made throughout my eight week tenure here. I vividly remember being unable to recall any of the reactions that I had done, to learning how to write them on my gloves, and finally being able to draw the structures of the compounds themselves from memory. Thin layer chromatography (RF values), separation using separating funnel (Partition coefficients), vacuum filtration, reflux, mass spec (molecular ion peak) and NMR spectroscopy - these were things whose theory we learnt in A-levels, but now I had the first hand experience of carrying them out in the labs.

6) At the end of the day, research in the labs has provided me with a different perspective on what goes on behind the scenes of every prescribed pill. I understand better how researchers working at the forefront of drug discovery would complement the very doctors who are the first line of contact for patients. And given a chance, I would love nothing better than to pursue this avenue of research to greater depth. Here's keeping my fingers crossed. Thanks for visiting my blog, and have a great day. Cheers!

Donal, Me, Dr. Griffith

Aptly arranged alcoholic aperitif => craic = 90

Beef goulash at AK Henry's today






Thursday, 22 June 2017

DAY 293/294

Jun 21 & 22

1) In the previous blog update I mentioned that we would conduct mass spectrometry to determine the identity of the second product that we created in the labs. So at 8.30am, Donal and I went over to York House, where he showed me how to use the mass spectrometer. After some initial dry runs, we inserted the sample into the machine and obtained the reading. Unfortunately, they did not match the product that we were looking for, much to our dismay.

2) So it was back to the drawing board. This time, I repeated the experiment, but followed an earlier (and similar) experiment carried out by Donal. We were half way through refluxing when we noticed something different about the DCM (dichloromethane/ methylene chloride) solution we were using. Strong hints of acetone were detected, suggesting that there were impurities present. This may have accounted for the change in mass spectra that we observed earlier in the morning. A quick TLC (thin layer chromatography) check confirmed that the product was indeed different, and hence we would have to (once again!) redo the experiment.

3) So I set up the experiment once more, making doubly sure to replace the tainted DCM solution with a fresh batch. We left the solution on low heat and reflux throughout the night. This morning, Donal had to present a research paper at DCU (Dublin City University), so I came alone to the labs to turn off the heating and carry out another TLC. This time things look a lot more positive. Hopefully our product will turn out fine, and we can proceed to the next step, which is to synthesize Deferasirox (DFX) from the two products that we have made.

4) In the afternoon, I went for my appointment with the Dublin School of Barbering, which offers free haircuts by their student barbers. To be honest, their quality is really good, and I can't really tell the difference haha. Anyway, I've spent the rest of the day back home, just contemplating life and wondering how to get everything packed up... That was today's blog update, and I hope you enjoyed it. Have a lovely day and thanks very much for visiting. Cheers!

That's a Nuclear Magnetic Resonance (NMR) instrument, used to determine the physical and chemical properties of atoms or the molecules in which they are contained.




That's me after getting a haircut 
(unfortunately there's no me before getting a haircut XD)


Wednesday, 14 June 2017

DAY 286

Jun 14

1) Today has been a tiring day for me. I got up early to meet Mr. Keogan in the labs. It seems I've underestimated how tiring it would be to work a 9-5 job, what with all the focus and concentration required haha. Luckily, we have informal tea and lunch breaks in between to boost our energy for the rest of the day.

2) In the morning, I helped Mr. Keogan to complete his own experiments (for his PhD), while learning many new analytical techniques. As an example, learning how to dry organic phase reagents using vacuum filtration apparatus and a rotary evaporator. Besides, we performed TLC (thin layer chromatography) which was taught in A-Levels! For other samples, we brought them for NMR spectroscopy (in York House, just opposite RCSI) for identification.

3) After lunch, we finally started with my experimental procedure. As of now, I need to do some more research on the availability of the reagents, or else some may need to be ordered. We got that far today, so here's hoping things will continue smoothly tomorrow. That's all for today, and I hope you enjoyed reading about it. Have a nice day, cheers!

A sneak peak in the labs...

Brunch

Lunch


Truth be told, I never imagined I'd be doing this :)