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One query:
In a high performance mass spectroscopic method while performing
bioanalytical method development and validation, if Column had been
changed from Hypurity Advance to Lichrospher RP-Select B,
Retention time, Flow rate, Injection volume, Aliquot volume and
reconstitution volume in sample processing method had been changed. I
want to know whether matrix effect, recovery will change or not.
I think these will change and we need to perform these activities
before finalizing our method.
Please give your inputs.
Regards,
Pragya Maheshwari,
QA
Clinsys,
Noida
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Matrix effect, recovery and such other parameters like selectivity of
the sample etc are parameters of your processing method and do not
vary when you change the column. when you change the column you may
observe a shift in the retention times or a change in the response of
the analytes or alterations in the peak properties. Matrix effect &
recovery remains constant for any amount of plasma aliquot taken or
amount of reconstitution solution added during your exercise.
Best wishes,
Santosh Tata
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The following message was posted to: PharmPK
Dear Nodia,
Matrix effect and recovery mainly depends on the extraction procedure.
If
you are using internal standard then it will not effect, however you
have
to re-validate the rest of the steps.
Dr Zafar
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Dear Pragya,
I think except plasma stability (freeze and thaw, bench top and
refrigerator), you need to repeat everything to fulfill full method
validation.
I assume, your linearity range doesn't change.
regards,
Jignesh
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The following message was posted to: PharmPK
Hi Pragya
The parameter that you mentioned (Matrix effect and recovery) will not
change by changing the column with respect to your processing method.
(Your processing method will remain same).
When you change the column you may observe a shift in the retention
times or a change in the response of
the analytes.
And to validate your column you can perform one P&A Batch that will
support your data.
Best wishes,
laxman kaswan
LifeSan Clinical Research (Centaur Pharma).
Bombay
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The following message was posted to: PharmPK
Recovery should depend on sample preparation procedure, before LC-MS/
MS analysis, as such it should not be affected by a column change.
However, in your message you also mention changing aliquot (is this
plasma volume?) and reconstitution volume; as these are part of the
sample preparation step I think recovery should be re-evaluated.
Matrix effect depends on your analyte co-eluting with some interfering
species, this is highly dependent on chromatography, therefore matrix
effect must be re-evaluated after a column change, as the two columns
could have different selectivities.
Patrice
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The following message was posted to: PharmPK
Dear Jignesh
I think the parameter like Matrix effect and recovery will not change
by changing the column with respect to your processing method.
(Processing method will remain same).
When you change the column you may observe a shift in the retention
times or a change in the response of the analytes.
To support your data or to validate your column you can perform
Partial validation.
laxman kaswan
LifeSan Clinical Research (Centaur Pharma).
Bombay
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Dear Laxman,
If I interpret Pragya's email correctly, she has changed following
highlighted parameters. With change in the stationary phase, there
will be change in matrix (peaks) elution order, which may interfere in
ionization. Secondly aliquot volume and reconstitution volume had been
changed, which may affect the loading on SPE cartridges/extraction by
solvent as well as effective solubilization on reconstitution (this is
with the case of higher processing volume compare to earlier method,
which has not been mentioned in her mail).
> In a high performance mass spectroscopic method while performing
> bioanalytical method development and validation, if Column had been
> changed from Hypurity Advance to Lichrospher RP-Select B,
> Retention time, Flow rate, Injection volume, Aliquot volume and
> reconstitution volume in sample processing method had been changed. I
> want to know whether matrix effect, recovery will change or not.
> I think these will change and we need to perform these activities
> before finalizing our method.
regards,
Jignesh
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The following message was posted to: PharmPK
A change in column could alter the matrix effect if a previously
separated matrix component now co-elutes.
If your sample aliquot volume has changed there is also the possibility
that recovery will be effected, depending on the extraction technique.
Basically if anything in your method changes, and it is a regulated
study, it's sensible validate the new parameters.
Regards
David
David Neville
Client Manager
Bioanalytical Sciences
Quotient Bioresearch
www.quotientbioresearch.com
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