Equipment & Manuals

Using the Analytical LCMS

A general guide on using the Analytical LCMS in G25 can be found here. The guide was prepared by Edwin G. Tse and Paul T. A. King and can be updated by anyone in the group. It serves as a walk-through for how to properly use the Analytical LCMS. This is not a substitute for proper training. Please check the lab job table to find the proper person to train you.

here is the LCMS sample preparation guide.

Using the Preparative LCMS

The operation of the preparative LCMS is identical to the analytical LCMS, with the addition of a fraction collector. A general guide on using the preparative instrument can be found here and was prepared by Edwin G. Tse. This is not a substitute for proper training.

LCMS Shutdown and Reboot

The LCMS should only be shut down in the case of extended time away from lab. When rebooting, it is imporant that things are done in the proper order. A quick guide to rebooting can be found here.

General Troubleshooting

A list of common issues encountered while using the analytical and preparative LCMS instruments can be found here. Where the fix is known, the solution is provided. If new issues are encountered while operating the LCMS instruments, it and its solution can be added to this list as a point of reference for the future.

Biotage Selekt

A general guide on using the Biotage Selekt in G25 can be found here. The guide was prepared by Yuhang Wang and can be updated by anyone in the group.

Biotage user manual can be found here.

Information on Biotage columns can be found here.

Write down your name and type of purification (i.e. normal or reversed phase) on the table affixed to the fumehood sash. Only write down your name if you are ready to run your purification, otherwise wait until you are closer to being ready.

There is no booking system and you can use the purification system as required, when it is not in use. There are currently 12 racks available.

Please don’t keep racks and tubes in your fumehood for prolonged periods of time. Combine your fractions as soon as possible after doing a column and clean the tubes thoroughly, finishing with several acetone rinses. Alternatively, transfer your tubes to a normal test tube rack (return later) and return the empty Biotage rack. Make sure there is no permanent marker on the tubes or on the rack. To ensure that the tubes dry quickly for the next user, place them upside down onto tissue on the bench or place them in the large drying cabinet at the back of the lab, before returning them to the Biotage or the designated cupboard.

We have bought many Sfär cartridges of varying sizes. You can reuse these several times by simply flushing with MeOH at the end of a run (to remove any impurities remaining on the column), followed by a less polar solvent. The column should then be dried by doing an air flush. As the Sfär columns contain spherical silica with a high surface area, they have a higher loading capacity. This means that you can use a smaller column than you usually would to achieve the same separation. Be aware that your compounds may behave differently on spherical silica in comparison to the standard Merck silica TLC plates we use. You may need to alter your gradient accordingly.

There are many methods of loading (i.e. liquid and dry) and you would have been sent a guide on this (speak to Fahima if you haven't). Once the silica has reached its lifetime (i.e. you start to see gaps between the silica and the frit) you can remove the frit and dispose of the silica. The empty cartridge can then be refilled as required.

If you need training on the instrument - contact the person in charge.