APR January/February 2022 - 53

« SPECTROSCOPY
Instrumentation: Handheld Raman
spectrometers included: TruScan RM (785 nm
laser), Progeny ResQ (1064 nm laser). FT-IR
analyses were conducted using a benchtop
Nicolet 8700 spectrometer.
Sample Selection
Samples consisted of seven suspect
unapproved dermal fillers that were taken
from an adjudicated criminal case, and were
labeled to contain cross-linked HA (24 mg/
mL), lidocaine HCl (3 mg/mL) and phosphatebuffered
saline (pH 7.0).
FT-IR Analysis
Standards Preparation
FT-IR spectra of neat standards were
collected.
Additionally,
the
spectra
Chloroform extraction: Approximately 0.3
mL of each liquid was placed in individual
4 mL glass scintillation vials. To each vial
was added 1 mL of deionized water and
the contents vortexed for 30 seconds, after
which 2 mL of chloroform was added to
the vial and centrifuged for 5 minutes at a
relative centrifugal force of gravity (RCF) of
3075 g. A portion of the chloroform layer was
transferred to a microscope slide and allowed
to air dry. The resultant semi-solid residue
was removed from the slide with a clean razor
blade, smeared on the IRE and examined with
no pressure applied for contact.
p
s
of
lidocaine HCl and lidocaine free base
recrystallized using chloroform were also
collected. Recrystallization was performed
to account for any variations or changes that
may be observed in the standard spectra due
to changes in crystallinity resulting from the
extraction process. Approximately 2 mg of
each standard was dissolved in chloroform
and used for each recrystallization. Several
drops of lidocaine dissolved in chloroform
were transferred to a microscope slide using a
disposable pipette and allowed to air dry. The
dried residue was transferred to the internal
reflectance element (IRE) surface using a razor
blade and fine-pointed probe. Appropriate
pressure recommended by the manufacturer
was applied and a spectrum was collected.
Sample Preparation
All samples were analyzed neat, oven dried
and extracted using chloroform, as described
below.
Neat analyses: Portions of suspect liquids
were transferred directly to the IRE surface
and a spectrum was collected with no
pressure applied.
Oven dried samples: Approximately 0.3 mL
of each suspect liquid was transferred to
individual microscope slides and placed in
the oven at a temperature of 90°C for 20
minutes. The solidified residue was removed
from the slide with a clean razor blade, placed
on the IRE and examined with appropriate
pressure applied for contact.
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www.americanpharmaceuticalreview.com |
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APR January/February 2022

Table of Contents for the Digital Edition of APR January/February 2022

APR January/February 2022 - Cover1
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APR January/February 2022 - Cover3
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