Download Quantification in Solid Mixtures

Quantification in Solid Mixtures
A Benchtop Solution for the Analysis of API and Drug Product
Quantification of components in complex solid
mixtures like formulated pharmaceuticals (drug
product) is crucial for the pharmaceutical industry
and generally in materials science.1 However,
the quantification of relative amounts of API
polymorphs and the corresponding amorphous
forms in the presence of excipients is not a
straighforward proposition. Current methods
include spectroscopic, thermometric and x-ray
techniques and often require laborious calibrations,
are expensive or may lack the required accuracy.
Designed to overcome these obstacles, Bruker’s
new solution enables easy and affordable
quantification of API polymorphs, drug loading
and amorphous content in solid mixtures. The
required instrument is a benchtop time-domain
NMR (TD-NMR), which can be deployed either in
a laboratory or a production environment.
Quantification by TD-NMR Benefits
„„Uses
a benchtop instrument: versatile, portable,
cryogen-free, small foot print, affordable and with low
maintenance costs
„„Minimal sample preparation: solid samples are placed
into the glass tube
„„Non-destructive technique: samples can be re-analyzed
or re-used for other purposes
„„High accuracy when sufficient signal to noise ratio
„„Selective, specially when observing 19 F, which is
typically not present in excipients
„„Push-button acquisition
„„Fast and easy calibration
„„Complete workflow from data acquisition to project
report with ability to export data in other formats for
additional processing
Stueber D. and Jehle S., Anal Chem, submitted
1
Innovation with Integrity
NMR
The new method uses 1H and 19F T1 saturation recovery
curves (SRCs) measured on a Bruker minispec mq20
benchtop TD-NMR instrument. For the analysis of a given
mixture, the SRCs for the relevant pure components, as
well as for the mixture itself, are measured. The relative
amounts of the mixture components are obtained from
a fit of the mixture SRC with a linear combination of
weighted pure component SRCs. For a two components
the equations is shown below.
© Bruker BioSpin 09/16 T161810
Where I is the intensity of the mixture, compound 1
and compound 2 at each recovery time point . S1 and
S2 are scaling factors which take into account number
of protons, molecular masses and plateau values of
the SRC curves. Modeling the mixture data yields the
concentration C1 and C2.
Bruker BioSpin
[email protected]
www.bruker.com