u/PostSpecific5119

Agilent 6470 Triple Quadrupole LC/MS - product peaks are moving and are thicker even though the test looked good

Hi :), I need help. I wanted to measure a Mixture of compounds on the Agilent MSMS. We always test them with our product, with the product we certified last year and sometimes Standalone solutions which contains certain compounds

of the mixture. The product is stored at -80°C and is pretty unstable. Since it's also pretty expensive we always test the method first. The test looks like this: we take one ampoule from our Mix and let it sit at room temperature until it is completely melted. We mix it with a vortexer for two minutes and put it in a crimp-top vial. After that we start the sequence. First there are two washing Injections with the same methods and after that it injects into a blank and after that into our product vial. Each method is 14 minutes long.

The test is just to check whether all components are present or if the method needs to be modified again. Since the test looked good and we could see all peaks we decided to start the entire sequence with the old product and the standalone solutions.

So the next day we started everything. The start is identical to the mix after that the mixtures are being warmed up in the hand so that they melt faster and being vortexes for two minutes again. The vials are being placed in the MSMS right before the machine injects the needle.

After everything was completed we checked the results and the peaks were thicker and the retention time was pushed back by approximately 1,5 minutes. We did another test with the exact same method and everything was fine again.

Edit: Tuesday: 1 test with two product injections

Wednesday: normal run with 4 wash injections of the product, 6 product injections, 6 old product injections, 6 of each standalone solution

Thursday: 1 test identical to the first test with one of the normal run vail

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u/PostSpecific5119 — 10 days ago