What You Can Achieve in a 6-Month Work Placement at Broughton Laboratories

I began my placement in Broughton Laboratories at the start of April and the last 6 months has flown by. After going through some basic volumetric and mass measurementtraining, reading a lot of Standard Operating Procedures and learning about Good Manufacturing Practice (GMP) in a working environment, I was put to work. I gained hands on experience in an analytical services laboratory and got to grips with GMP documentation and pharmaceutical analysis. After some HPLC and data processing training, I was allowed get started on the project that drew me to Broughton Laboratories in the first place – Method development and method transfer from HPLC to UHPLC.

Collaborating with Thermo Fisher Scientific, we were working on the Vanquish Flex – a highly sensitive and accurate piece of kit. With high pressure capabilities of over 1000 bar and solvent savings of over 70% on average, it’s an ideal piece of kit for the modern day analytical laboratory.

In my last blog, I talked about the two main projects we undertook to transfer to the Vanquish Flex. The first project was developing a method for the detection of Carbonyls in e-liquid aerosol. A list of 16 different carbonyls and ketones was drafted; some mandatory for identification and others just desirable. At present, 13 of the 16 carbonyls have been identified with the remaining three causing some challenges. Due to the complex nature of e-liquids, with various flavourings and scents, analysing the final three components of the sample is proving difficult. Further research and work will be required in order to fully develop this method.

The second method discussed was for Ibuprofen – this involved taking the method for Ibuprofen Tablets as outlined in the British Pharmacopeia and transferring this to UHPLC. Impurity B and Impurity E were of particular interest to us, as these are outlined as the main impurities of interest in the Pharmacopeia. Much method development was carried out in order to optimise the method by reducing run time but mostly, improve the resolution between the Ibuprofen, Impurity E and Impurity B. The following method was developed.

 

Table 1: Optimisation for Ibuprofen Method

 

  Original HPLC Method

  Optimised UHPLC Method

Column

Nucleosil C18,

250mm x 4.6mm (i.d.), 10µm

Hypersil Gold Vanquish,

100mm x 2.1mm (i.d.), 1.9µm

Mobile Phase

Composition

75% Methanol, 22% Deionised

Water, 3% Phosphoric Acid

45% Acetonitrile, 55%

Deionised Water, pH adjusted

to 3.0 with Phosphoric Acid

Flow Rate

1.5 ml/min

1.0 ml/min

Temperature

25°C

55°C

Injection Volume

20µl

1µl

Run Time

10 minutes

4.5 minutes

Pressure

~250 bar

~660 bar

 

Although far higher in pressure, this method gave much better resolution between impurity B and Ibuprofen; previously, Impurity B was a rider peak upon Ibuprofen and now has a resolution of 2.14. Resolution between impurity E and Ibuprofen was increased by over 300% - from 1.84 to 6.16. The width of the Ibuprofen peak was reduced from 0.21 minutes to 0.03 minutes and the asymmetry of the Ibuprofen peak still falls within parameters of the British Pharmacopeia. Column efficiency went from just under 4,000 plates to well over 15,000 – over 300% increase.

After 6 months, I have grown very fond of working in Skipton and its picturesque setting in North Yorkshire. I was lucky enough to be given a true welcome from my colleagues and look forward to keeping in contact with them. I have gained so much knowledge and practical experience from working in the GMP analytical services laboratory and really gained a feel for HPLC and UHPLC in my work on method development. Although I am heading back home to finish out my Masters in Analytical Chemistry and start my career in Ireland, I look forward to the time I can return back to England and in particular, to Broughton Laboratories.

Posted by Eilin Ni Chroinin | Oct 17, 2017 12:15:00 PM | Categories: Insider

Eilin Ni Chroinin