r/massspectrometry

Help with SRM Method

Hello I was wondering if anyone could help me figure out what is wrong with my SRM method. When I run a full scan on my pesticide sample (picture 1) there are two distinct peaks for Endrin and Dieldrin. However after I set up my SRM method using the ions with the highest intensities, both peaks basically disappear (picture 2). I have tried to develop this method using transition pairings from literature I've found from our standard supplier as well as from ThermoFisher and I still encounter the same issues. Both scans were done with the exact same instrument method so I think it's pretty safe to rule out instrument settings. If anyone has any ideas please let me know.

u/MobilePhase1987 — 2 days ago

Is ZIC-pHILIC (5 micron) 50mm x 2.1mm better for metabolomics than ZIC-HILIC (3.5 micron) 100mm x 2.1mm

As title. I am in a situation where I have to choose one of these two for procurement without option of trail runs. Hence I need expert opinion.

What would be better got global untargeted metabolomics (Ultimate 3000 + Exploris 120 setup)?

I am a metabolomics noob. Please guide me. Both are 100 Angstrom.

I would be using it to do C13 tracer based work on mmmalian cells (after I gain expertise in basics, of course)

I also have option for ZIC-pHILIC (5 micron) 100mm x 4.6 mm

So my options are

ZIC-pHILIC (5 micron) 100mm x 4.6 mm

ZIC-pHILIC (5 micron) 50mm x 2.1 mm

ZIC-HILIC (3.5 micron) 100mm x 2.1 mm

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u/bluemooninvestor — 2 days ago

Interpreting GCMS results from drugs?

Results from the PAGroundhogs.org harm reduction lab.

Is there a way to quantitate the amount or at least percentage of each component?

Edit. Thanks! Sorry if this is not allowed.

u/Silly_Bath7019 — 3 days ago

Can anyone help identify this compound?

SPME-GC/MS of Vermont maple syrup, RI of 917 on a 30M DB-5MS

Looks like a furanone of some kind that makes up 3.5% of the VOCs but it's not in any of my libraries. 😭

Ion [m/z] Intensity Intensity [%]

36.6 1024.0 3.8438

37.8 2385.0 8.9527

38.8 12475.0 46.8281

39.8 26640.0 100.0000

40.8 4787.0 17.9692

41.8 1953.0 7.3311

42.8 11368.0 42.6727

43.8 1422.0 5.3378

44.8 3285.0 12.3311

52.6 570.0 2.1396

54.6 1257.0 4.7185

55.6 234.0 0.8784

67.8 22952.0 86.1562

68.8 3673.0 13.7875

70.4 364.0 1.3664

83.6 618.0 2.3198

96.4 354.0 1.3288

111.8 18488.0 69.3994

Ohgodredditdestroyedmyformatting

u/WahWash — 4 days ago
▲ 22 r/massspectrometry+1 crossposts

I need help with MS

Hi everyone

My current lab wants to acquire an LC-MS/MS spectrometer, and I've been chosen to learn everything about it and implement the methodologies. The problem is that no one in the lab knows anything about mass spectrometry and I was the only one selected to learn. As you can imagine, I'm quite lost, and I'd like to know where I can find information to study or familiarize myself with this equipment, as it's very expensive, and I don't want to end up breaking something or wasting money.

Thanks in advance

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u/pallmallrosao — 7 days ago

Peptide intact-mass check: expected charge envelope plus a persistent +22 Da series

I am reviewing an ESI intact-mass run for a synthetic peptide. The deconvoluted neutral mass matches expectations within tolerance, and the raw spectrum shows the expected multiply-charged envelope. A second, lower-intensity series appears consistently about +22 Da relative to the corresponding charge states. My first thought is a sodium adduct, but I want to rule out a deconvolution artifact or a sample-preparation issue before including that in the report. The blank is clean, the series weakens after fresh desalting, and it is more prominent in one buffer. Would you confirm the assignment through exact spacing across charge states, targeted MS/MS, alternative adduct conditions, or a different deconvolution setup first? Also curious how you report identity confidence when the main mass is correct but adducting is obvious.

u/Primary_Tailor30 — 8 days ago

Why Agilent Q6520 instrument vacuum worsen when instrument cover is in place

This is happening after the smart card stopped working and is replaced with a used one. The vacuum couldn't reach the same as before even after long time pumping. Now the vacuum achieved with the cover off is close to what the system can achieve before with cover in place, but the vacuum will worsen if the cover is put back on and slowly climbing. I have put the cover back on long enough time to see if it eventually fail the criteria for getting the instrument ready. I understand there might be offgassing from the chamber under the trapped heat when the cover is closed, but that should be the same as before the replacement. I am wondering if there is some kind of control mechanism that is still not working properly due to the smart card replacement. Anyone have any thought on this? Thank you.

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u/Training_Pangolin177 — 8 days ago

Single HRMS for both small and large molecule applications (Waters Xevo qTOF)?

Hi there,

I am specialized in the small molecule world, and have never touched anything large molecule. Now, my manager wants us to start analyzing large molecules, from peptides, polysaccharides, to complex polymers. We are a small lab and only have HPLCs, a single quad GC-MS, and a HRMS (Waters Xevo G2-XS). My question is the qTOF. We still use this for small molecule needs (mainly impurity screening and residue analysis). I know that Xevo can be used for both small molecule and large molecule analyses but I thought that it is generally dedicated to one way, not both. Is there anyone who uses single instrument for both small and large molecule applications and switch them frequently?

I am specifically asking if anyone does this on a Waters HRMS. Years ago, when I had a training on a Synapt, the trainer told me that she would not recommend to use Synapt for both applications because the Waters calibration solution mix for large molecule has a component (I don’t recall exactly but somewhere below m/z 200) that sticks to the instrument and could cause a calibration issue when switching back to the small molecule application. I wonder if that’s true. I would love to hear your experience on a Xevo qTOF. Thanks!

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u/Aska2020 — 8 days ago

Xevo G3 QToF – Strong background peak preventing calibration even with infusion OFF

Hi everyone! I’m troubleshooting a Waters Xevo G3 QToF and I’m having an issue that is preventing us from calibrating the instrument.

We are trying to calibrate with our usual calibrant, but there is a very strong background peak already present even before we introduce the calibrant. The background signal is strong enough that the calibrant peaks are overwhelmed/interfered with, so we cannot get a proper calibration.

The situation is:

  • LC flow is OFF
  • Sample infusion is OFF
  • LockSpray infusion is OFF
  • Both Sample Flow Control and LockSpray Flow Control show “Idle”
  • Sprayer position = Sample
  • However, we can still see what appears to be a continuous spray from the sample sprayer
  • There is a strong signal on the QToF even though we have not infused calibrant or sample
  • The major unexpected signal appears around m/z 60
  • The signal is strong enough that when we try to introduce the calibrant, the background peak overwhelms the calibrant signal and we cannot calibrate properly

Current Fluidics settings are:

Sample Flow Control

  • Infusion flow rate: 5.0 µL/min
  • Flow state: Infusion
  • Reservoir: C
  • Status: Idle

LockSpray Flow Control

  • Infusion flow rate: 10.0 µL/min
  • Flow state: Infusion
  • Reservoir: B
  • Status: Idle

Sprayer position: Sample

I understand that the displayed “Flow State: Infusion” does not necessarily mean the pump is actively running because the actual status is Idle.

What is confusing us is that we appear to have continuous spray/background signal despite both fluidics being Idle.

Our main concern is that this is preventing calibration. We don't want to start replacing valves, tubing, or other consumables without knowing what is actually causing the problem.

Has anyone experienced this on a Xevo G3 QToF?

Could this be caused by:

  • A fluidics valve not switching completely?
  • IPA/wash solvent leaking or being routed to the sample sprayer?
  • Residual pressure/solvent in the fluidics line?
  • A divert-valve or fluidics routing issue?
  • A problem with the sample fluidics pump/valve?
  • Or could the strong m/z ~60 signal be coming from another source entirely?

What would you check first, and is there a way to completely stop/isolate the sample fluidics so we can determine where this signal is coming from?

I’ve attached a screenshot of our current Fluidics/Tune page. Any advice from anyone familiar with the G3 would be greatly appreciated.

https://preview.redd.it/q0mqd9x60zih1.png?width=1132&format=png&auto=webp&s=b6720caa743614890b9edf541d9ccf02c97d719f

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u/chomkycinnamonrolls — 8 days ago
▲ 8 r/massspectrometry+1 crossposts

how to diagnose Agilent 1290 high speed pump A problem?

It doesn't build pressure. Initially the pressure would go up to 150 bar in pressure test and do the jigsaw thing before quit, tried sonicating all the valves in water and IPA, intially it help a little, which means only less of jigsaw, but still never was able to build pressure above 150, after long time sonicate in 50C water and put back together it's even worse. How to tell what is the problem? Doesn't seem to be seal since it is not leaking, but which valve? Primary inlet, outlet or secondary outlet valve? Or more than one?

u/Training_Pangolin177 — 11 days ago
▲ 7 r/massspectrometry+1 crossposts

Is a helium leak detector really necessary for GC-MS?

Do you really need a helium leak detector when changing a helium cylinder for GC-MS?

We normally check the regulator and fittings after a cylinder change, but I’m wondering if buying a dedicated helium leak detector is actually necessary for routine use.

Do most GC-MS labs use one?

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u/zeydullak — 10 days ago

Accidentally left the oven baking at 325 overnight

So as the title said… I left my gcms oven baking overnight at 325 and forgot to turn it back at 55. I usually do baking when there is high air/water or column is newly changed but I did it bc of the air/water leaks.

I did search online and says it is safe as long as it is under or at the limit of manufacturer but i also saw that phenomenex only recommend 1-2hrs when you bake.

Based on your experience (if you encountered this), does it affect my gcms? Should i clean the ion source again and change filaments just in case it was busted?

Thanks

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u/userisanon_ — 12 days ago

Can you suggest mobile phase

Hey team, recently involved in development of simultaneous estimation of Indacaterol and Glycopyrronium

Any suggestions for mobile phase ??

Isocratic

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u/rameshPM — 10 days ago
▲ 9 r/massspectrometry+3 crossposts

WIRE FRAUD / THEFT ALERT - STAY AWAY FROM CMION Service Engineer in Bay Area! They have committed Grand Theft upwards of $100,000 for a Sciex 4500 I purchased from them.

I bought a Sciex 4500 LCMSMS from Jay Ambrosio & Dae Cho of CMION in San Leandro, CA. I wired them in full because I had just purchased a Sciex 5500+ from them 2 months prior with no issues. A week and a half after they accepted my wire, and one day before installation was scheduled, Jay told my company that he was canceling the transaction because I wasn't using CMION for the installation & service contract. I had already hired my favorite engineer months prior and had prepaid him. Jay threw a tantrum, saying he won't allow other service engineers to work in 'HIS TERRITORY' - the Bay Area. Delusional! They have not refunded me after almost a month and continue to keep the instrument that is legally owned by my company. They are trying to sell the 4500 I bought on eBay.

u/WaviLab — 13 days ago

How important is temperature uniformity in circulating water baths?

In laboratory applications, maintaining a stable temperature throughout the bath can be just as important as reaching the target temperature.

For those using circulating water baths:

  • How do you verify temperature uniformity?
  • Have you experienced temperature differences within the bath?
  • Does circulation significantly improve your results compared with a standard water bath?
  • What temperature range do you typically work with?

Would be interested to hear experiences from lab and QC professionals.

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u/Which_Lifeguard_864 — 14 days ago