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A Validation Week

Sometimes I think that having a holiday is what you need to guilt you back into working. Last weekend I went home (together with 3 friends from Ireland) for an extended weekend. I really enjoyed showing them the sights of Malta, and also meeting my sister who came over too. However once I got back into the lab I knew that I needed to get down to business. Since the Mass Spec is still not working (still waiting for the parts to arrive), I decided to make use of the HPLC part of the LC-MS instrument. Usually you are not allowed to make use of this front end portion of the instrument on its own. However since the MS part was not working I got permission to use it. Therefore this gave me time to work on my method’s transferability to the actual instrument I will be (hopefully) using.

Before my trip I had ascertained that the method transfers quite well, and I was pleased with the preliminary results. However I knew that as with any method this needs to be validated. Therefore on my return I started working on this section of the process. I have now finished the validation of the HPLC method and I am quite pleased with the overall results. I did have to remove an analyte from the 11 I had started with, since it did not validate in any test. But I am not too concerned about that. After all that is why I started with 11. My supervisors had initially told me not to go for more than 5 analytes, but I had argued that it is better to start with more, and then eliminate later on, depending on the results.

I certainly hope that the parts arrive soon, and that the instrument is fixed very soon. In the meantime, I have figured out what I could do to ‘fill the time’. The parts have been said to be delivered either yesterday (so no) or early next week. I desperately hope that these parts are the actual ones required and that once it is fixed it keeps working. Another girl who is finishing her PhD will probably get onto the instrument first. But as long as it is working there is hope.

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Mass Spec Woes

May 20, 2011 3 comments

As part of my research I need to get access to an LC-MS. I have carried out most (all?) of the work I could do on the HPLC part and have been waiting to get onto the Mass Spec. Unfortunately this instrument is quite old and does not work well it seems. I have been hearing tales of horror about it from previous researchers using it, and it seems that the cycle repeats. It had been down since the beginning of March and they just got it to work again this week. I was supposed to get trained on it next week, but today I received an email saying that something else came up and it will be out for another ‘couple of weeks’.

I find this to be extremely frustrating, as I cannot progress in my research without this piece of equipment. I will hopefully go talk to my supervisors next Monday or so, and see how to proceed. One of the suggestions might be to go to another University and get access to their Mass Spectrometer. But generally these instruments are quite in demand, so to get access to one might not be that easy. I will see how this goes. Without it, I am not too hopeful about the future of my PhD.

Well, as you can see, I am not in the greatest of moods. I have been waiting to get access to the Mass Spectrometer for a couple of months now, and if only it worked, I would have progressed quite a bit I would hope.

Wish me luck!

Another Week is Over

February 27, 2011 Leave a comment

The past week has been a hectic week PhD wise. I had a conference on Monday and Tuesday, a meeting with my supervisor on Wednesday and lab demonstrations on Thursday. In addition I have been working to develop my HPLC Method. I have spoken about the conference and lab demonstrations previously. I have also touched upon the HPLC method development.

The method development has been progressing slowly but steadily. If things keep on progressing the way they are I would be indeed quite happy. I tried out some things suggested by a girl I met at the conference last Tuesday, and things have improved. I did some more runs yesterday (yes I know it was a Saturday) and got the results this morning (yes it is a Sunday), and I am quite pleased with the way things are progressing, though 1 peak is still missing/it peeks out a bit from behind another, so that it on my agenda for tomorrow. The R squared values for the calibration curve I did are all greater than 0.99, so not too bad, though there is room for improvement. Once I (hopefully) separate my current 6 peaks, I will then need to add in another 5 compounds (ordered this week 🙂 ), and then start working on joining the HPLC method to the sample preparation technique and the Mass Spec analysis technique. So still a way to go to be able to start collecting samples for analysis. But we will get there.

I also had a meeting with my supervisor on Wednesday. We generally have lab meetings every Thursday, but since I am demonstrating all day Thursday, I will be having meetings with my supervisor every now and then depending on need, until I finish demonstrating. During the meeting we discussed a couple of things I had been meaning to talk to her about, in particular things which do not lend themselves well to discussing during a lab meeting.

First up was the thing I was dreading most. I had given her my literature review a couple of weeks ago (just before she went on holiday, and she read it during her holiday). I was quite pleased with the feedback however. She said it was quite good for a first try (that is what we aim for after all), and she gave me a couple of changes to make. I have now carried out all the minor changes, and will start focusing on the sections which involve searching for more data and so on. The main issue I need to do is to summarize  everything  at the end, rather than simply saying what other people said, without giving any opinions, and therefore this leaves everything hanging a bit. She also noticed my love of the words therefore, nevertheless etc, and was told to cut down on those. The last part of the meeting consisted of me discussing some points I wanted to talk to her about, such as ordering of the new chemicals, how my progress is getting along, the conference details, and lastly, but quite importantly for me, we discussed time off. I now have approval for my days off till the end of August. It feels good to know roughly when I can get to go home etc etc.

Overall, a busy but pleasant week. I could do with it being slightly less hectic, but rather a week like this one, to a slow week, or one when nothing goes well.