A heterocyclic drug with 2 nitrogen atoms in the rings is analysed on Waters Alliance 2690 (stainless sample loop). A Supelco Discovery Amide C16 is used. The mobile phase is 25 mM phosphate/10 mM dimethyloctylamine pH 7.4 (at pH 3 the drug has no fluorescence). The problem is that a peak always appears at the RT of the drug when a relatively concentrated sample is injected, even after extensive wash with mobile phase, after injecting mobile phase 15 times and/or needle wash. It is suggested that the drug stick to the stainless sample loop and a PEEK loop be used. Has anyone seen this problem before? Any suggestions will be greatly appreciated.
MAny thanks.
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By anomymous on Thursday, September 7, 2000 - 06:09 pm:
I have never seen anything stick to a stainless steel loop, while I have seen stuff stick to PEEK frits or the rotor seal in a Rheodyne injector. On the other hand, none of this should apply to the standard Alliance injector. How do you do the needle wash in this system?
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By Anonymous on Monday, September 11, 2000 - 01:25 pm:
What is the sample dissolved in? Are your sample and mobile phase compatible? Is there any possibility that precipitation is occurring in the sample loop?
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By Anonymous on Monday, November 20, 2000 - 01:28 am:
It is known, that 316ss (or metal in general) has caused sample components of very polar nature to 'stick' - see certain pesticides; this can also happen in other parts of the sample injection area like the valve seal; what about metal frits in the column ?
Have you thought about residual components from previous injections contaminating the injector or parts around the injection point ? What about a service of the injector ? Injectors must be serviced dependent on the usage . No car would run without an oil check once in a while.
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By Anonymous on Wednesday, November 29, 2000 - 06:26 am:
As Waters suggested, I switched to Waters 717 autosampler (previously Alliance 2690). The problem was solved.
Thanks a lot for your imput.
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