Dear members,
I have two questions about my work,
1)If is there competition to product adduct H+or Na+?
2)Why the TIC peak after column dissapeared comparing with directly flow injecting ? what factors should I consider to solve this question?
Thank you in advance.
Michelle
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By Anonymous on Friday, March 12, 2004 - 10:02 am:
To answer the first question: There is competition between the formation of H+ and Na+. Increasing source CID or temperature can shift formation toward M+H+ and away from Na+ or other adducts. (Adducts form under lower energy conditions.)
I am a little unclear about the second question. Are you saying that you don't see any peak corresponding to your analyte? Or are you saying that M+H+ disappears?
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By Anonymous on Sunday, March 14, 2004 - 09:57 pm:
Dear Anonymous,
I can describe in detail. I run a sample through the column firstly and there is no any TIC peak in the chromatograph and any corresponding Mass spctra. Then I injected the sample to Mass directly, Mass gave me some information same with my expection. My collegue said this result was due to diffusion in column and flow. I cann't agree with her.
So could you give me more direction?
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By Anonymous on Sunday, March 14, 2004 - 10:00 pm:
Dear Anonymous,
I can describe in detail. I run a sample through the column firstly and there is no any TIC peak in the chromatograph and any corresponding Mass spctra. Then I injected the sample to Mass directly, Mass gave me some information same with my expection. My collegue said this result was due to diffusion in column and flow. I cann't agree with her.
So could you give me more direction?
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By Anonymous on Monday, March 15, 2004 - 05:30 am:
Are you sure that your analyte is eluting from the column? What is your mobile phase? When you inject the sample into the MS, and you using mobile phase at a flow equivalent to the flow from your column, or is it just the analyte and solvent?
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By Anonymous on Monday, March 15, 2004 - 05:19 pm:
Yes, I am sure. I just inject the sample to MS directly during the same run as injecting to LC.
No any condition was changed. I use Waters 2695-ZQ.And the sample is ionic sample so I think it could be elunt between 30 min.
Any comment?Thank you.
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By Kostas Petritis on Tuesday, March 16, 2004 - 10:16 am:
Hi Michelle,
If I understand well, in flow injection analysis (FIA) where you injected your sample without column, you observe a [M+Na]+ ion as the major ion; which desappears when you inject in your LC column before detection with the MS.
My first guess is that when you are doing FIA, you have plenty of Na+ available to create adducts, that is why you see your [M+Na]+. In the LC version (and assuming that your compound of interest is retained a little bit) most of the Na+ will be eluted in the hold up time, so when your analyte is eluted it has not enough Na to form the adduct and maybe the [M+H] is your major peak (or maybe you see nothing because your compounds is not easily ionisable).
Hope the above helps,
Kostas
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By Anonymous on Tuesday, March 16, 2004 - 02:37 pm:
Is your method isocratic? If this is the case, how do you know that your compound elutes from the column? Do you only think it elutes?
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By Anonymous on Thursday, March 18, 2004 - 08:31 pm:
Thank you, Kostas, however, you give me
a direction to identify the cause.
And Anonymous: I run my sample isocratic. The sample is easy to ionize so I think it should be elute in thirty minuts.
I will post my continuos observation, pls give me more in future.
Michelle
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By Anonymous on Friday, March 19, 2004 - 03:13 pm:
I bet that you problem is that the compound either does not elute under your isocratic conditions or that the peak is so wide that you do not recognize it as a peak. Try a gradient and see if you still dont find your peak.