Development and validation of an LC-MS/MS method for the simultaneous estimation of tadalafil and macitentan in rat plasma: Greenness assessment and design of experiment approach
Green Analytical Chemistry,
Journal Year:
2025,
Volume and Issue:
unknown, P. 100211 - 100211
Published: Jan. 1, 2025
Language: Английский
Development of a Quality by Design-Based Ultra-Performance Liquid Chromatography Method for the Simultaneous Estimation of Casirivimab and Imdevimab with Greenness Metrics
Sravanthi Gandu,
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Kumaraswamy Gandla
No information about this author
Green Analytical Chemistry,
Journal Year:
2025,
Volume and Issue:
unknown, P. 100248 - 100248
Published: March 1, 2025
Language: Английский
Quality by design-based optimization and HP-TLC densitometric standardization of Theobroma cacao L. extract as a nutraceutical supplement
Atith Muppayyanamath,
No information about this author
Darasaguppe R. Harish,
No information about this author
Vinayak Mastiholimath
No information about this author
et al.
Frontiers in Nutrition,
Journal Year:
2025,
Volume and Issue:
12
Published: April 9, 2025
Our
previous
studies
identified
the
hydroalcoholic
extract
of
defatted
Theobroma
cacao
L.
bean
(CE)
as
a
cancer-preventive
and
protective
agent
against
chemotherapeutic-induced
toxicities,
specifically
doxorubicin-induced
heart,
liver,
kidney
toxicities.
An
analytical
method
for
phytochemical
standardization
was
developed,
acute
oral
toxicity
studied
in
female
Wistar
rats
following
OECD
423
guidelines.
In
brief,
CE
extracted
using
an
80:20
alcohol-water
(%
v/v)
mixture
through
cold
maceration,
followed
by
spray
drying
to
obtain
powdered
CE.
Utilizing
Quality
Design
(QbD)
approach
with
Expert
(DoE)
software,
we
optimized
tablets
via
direct
compression.
The
central
composite
design
(CCD)
included
five
center
points,
Avicel
PH
-
101
croscarmellose
sodium
(CCS)
factors,
disintegration
time,
hardness,
%
loss
due
friability
measurements.
Among
13
formulations,
batch
F-9
emerged
one
within
space,
containing
35%
5%
CCS.
formulation
exhibited
time
5.2
min,
hardness
4.2
kg/cm2,
0.34%.
Importantly,
no
toxic
effects
were
found
at
2,000
mg/kg
study.
contains
vital
bioactive
polyphenols,
including
(-)-epigallocatechin-3-gallate
(EGCG)
(+)-catechin
(CTN).
We
developed
marker-based
HP-TLC
densitometric
analysis
mobile
phase
9:9:2
v/v
[ethyl
acetate:
toluene:
formic
acid],
which
revealed
CTN
Rf
0.49
EGCG
0.23.
This
validated
according
ICH
requirements.
conclusion,
novel,
simultaneously
detects
cocoa
extract.
Tablets
formulated
compression
are
safe
nutraceuticals
hold
promise
supplements
palliative
cancer
therapy.
Language: Английский
Analytical Quality by Design (AQbD) Principles in Development and Validation of Stability‐Indicating RP‐HPLC Method for Simultaneous Estimation of Diltiazem HCl and Eugenol in Nanoethosomes
Purva Usgaonkar,
No information about this author
Anjana Adhyapak,
No information about this author
Rahul Koli
No information about this author
et al.
Separation Science Plus,
Journal Year:
2024,
Volume and Issue:
unknown
Published: Sept. 28, 2024
ABSTRACT
The
study
developed
and
validated
a
robust
reverse‐phase
high‐performance
liquid
chromatography
(RP‐HPLC)
method
for
simultaneous
estimation
of
Diltiazem
HCl
Eugenol
in
nanoethosomes
using
analytical
quality
by
design
(AQbD)
principles.
optimized
utilized
mobile
phase
methanol
0.1%
Orthophosphoric
acid
(OPA)
50:50
%
v/v
ratio,
with
flow
rate
1.0
mL/min
isocratic
elution
on
Phenomenex
Luna
C‐18
column
(5
µm,
150
mm
×
4.6
mm)
at
30°C.
This
setup
resulted
retention
times
6.838
min
23.135
Eugenol.
Validation
followed
International
Council
Harmonization
(ICH)
Q2
(R1)
guidelines,
demonstrating
excellent
linearity
correlation
coefficients
0.9982
0.9991
across
the
5–25
µg/mL
range.
limits
detection
(LOD)
were
1.341
0.960
Eugenol,
quantification
(LOQ)
4.065
2.912
µg/mL,
respectively.
Stability
testing
under
acidic,
alkaline,
oxidative,
thermal,
photolytic
conditions
adhered
to
ICH
Q1A
(R2)
Q1B
guidelines.
AQbD‐based
is
effective
routine
analysis
bulk
pharmaceutical
dosage
forms,
fully
complying
standards.
Language: Английский
Advanced stability-indicating gradient elution reverse phase-high performance liquid chromatography method development and validation for simultaneous estimation of rutin and curcumin using an analytical quality by design approach
Daneshwari Bhusannavar,
No information about this author
Bhuvaneshwari R. Sharannavar,
No information about this author
Rahul Koli
No information about this author
et al.
Analytical Chemistry Letters,
Journal Year:
2024,
Volume and Issue:
14(4), P. 607 - 621
Published: July 3, 2024
AbstractThis
research
delves
into
a
systematic
Analytical
Quality
by
Design
(AQbD)
approach
to
develop
and
validate
stability-indicating
robust
RP-HPLC
method
for
the
simultaneous
determination
of
Rutin
Curcumin,
compounds
known
their
anti-inflammatory,
antioxidant,
wound-healing
properties.
Utilizing
QbD
principles,
critical
parameters
(CMPs)
were
identified
screened
using
design
experiments
(DoE)
optimized
via
response
surface
methodology
(RSM)
with
Central
Composite
(CCD).
The
chromatographic
separation
used
Phenomenex
Luna
C18
column
gradient
elution,
methanol
0.1%
formic
acid,
flow
rate
1
ml/min,
detection
at
345
nm
(isosbestic
point).
retention
times
5.63
mins
17.01
Curcumin.
stability
indication
developed
HPLC
was
performed,
validation
meticulously
conducted
following
ICH
Q2(R1)
guidelines,
demonstrating
linearity
over
2-10
μg/ml
5-25
correlation
coefficients
0.9999
0.9998,
respectively.
Precision
studies
showed
%RSD
within
acceptable
limits,
accuracies
ranged
between
97-100%.
This
validated
offers
reliable,
sensitive
quantifying
suitable
routine
analysis
in
pharmaceutical
laboratories
quality
control.GRAPHICAL
ABSTRACTDisplay
full
sizeKeywords:
designReverse-phase
high-performance
liquid
chromatographyCentral
composite
designRutinCurcumin
Supplementary
informationFigures
S1-S3
are
given
supplementary
file.
Language: Английский
Secondary Metabolite Fingerprinting and Antioxidant Potency of Eleusine indica: An Integrated Chromatography and In silico Investigation
International Journal of experimental research and review,
Journal Year:
2024,
Volume and Issue:
40(Spl Volume), P. 245 - 255
Published: June 30, 2024
Natural
regimens
and
constituents
serve
as
the
primary
sources
for
drug
conservation,
each
herbal
regimen
possesses
unique
ethnomedicinal
biological
properties.
Therefore,
researchers
are
currently
more
interested
in
exploring
activity
of
existing
plant
species
with
most
systematic
approach
to
be
used
specific
therapeutics
proposed,
either
crude
extracts
or
bioactive
metabolites.
The
present
study
also
explores
antioxidant
potency
ethanolic
Eleusine
indica
(a
weed
an
agricultural
field)
through
chemical
fingerprinting
analyses
high-performance
thin-layer
chromatography
(HPTLC),
followed
by
gas
chromatography-mass
spectrometry
(GCMS)
silico
investigation
a
way.
Briefly,
this
aims
observe
presence
secondary
metabolites
associated
activity.
After
extraction,
fingerprint
was
carried
out
mobile
phase
consisting
ethyl
acetate,
acetic
acid,
formic
water
ratio
10:1.1:1.1:2.3
volume,
where
than
eight
fluorescent
non-fluorescent
bands
were
found,
highest
density
peak
area
at
Rf
0.87
lowest
0.18.
As
per
GCMS
report
E.
composed
several
Further,
based
on
higher
value,
we
have
selected
seven
(EI_1
EI_7)
that
constitute
molecular
docking
against
three
target
enzymes:
cyclooxygenase-2
(PDB
ID:
5F1A),
peroxiredoxin-5
1HD2),
haemoxygenase
1
3CZY)
assess
potency.
Overall,
results
revealed
EI_7
(2,7-dioxatricyclo
[4.4.
0.0(3,8)]
decane-4,5-diol)
showed
similar
ideal
drug-ability
profiles
ascorbic
acid
considered
lead
further
therapeutic
use
complementary
agent.
Language: Английский
Stability‐Indicating RP‐HPLC Method for Lopinavir Estimation in Pharmaceutical Co‐Crystals: A Design of Expert Approach
Pranali Mehta,
No information about this author
Bhuvaneshwari R. Sharannavar,
No information about this author
Rahul Koli
No information about this author
et al.
Separation Science Plus,
Journal Year:
2024,
Volume and Issue:
unknown
Published: Nov. 19, 2024
ABSTRACT
The
primary
objective
of
this
investigation
was
to
develop
and
validate
a
robust
reversed‐phase
high‐performance
liquid
chromatography
(RP‐HPLC)
method
for
the
quantification
lopinavir
in
co‐crystals
formed
with
fumaric
acid
acetamide.
A
Box–Behnken
design
within
experiment
framework
employed
optimize
chromatographic
conditions.
utilized
Phenomenex
Luna
C18
column
mobile
phase
methanol
0.1%
formic
(80:20
v/v)
at
flow
rate
1
mL/min,
detection
259
nm.
Validation
followed
ICH
Q2
(R1
R2)
guidelines,
confirming
method's
specificity,
accuracy,
precision,
linearity,
robustness.
Co‐crystals
were
prepared
using
liquid‐assisted
grinding
reaction
crystallization
techniques.
validated
HPLC
successfully
quantified
these
co‐crystals,
recovery
rates
ranging
from
96.3%
99.8%.
Forced
degradation
studies
under
various
stress
conditions
(acidic,
base,
oxidative,
thermal,
photolytic)
demonstrated
capability
distinguish
its
products.
In
conclusion,
developed
RP‐HPLC
is
suitable
routine
analysis
quality
control
co‐crystal
formulations.
This
not
only
provides
precise
but
also
offers
insights
into
enhanced
delivery
potential
through
co‐crystallization,
contributing
improved
therapeutic
efficacy
HIV/AIDS
treatment.
Language: Английский
Development of marker-based quantification methods fo r Diospyros Montana Roxb using DoE approach and in-silico anti-diabetic screening of selected phytoconstituents of the Diospyros genus
Ashwini M. Kambalyal,
No information about this author
Parixit Bhandurge,
No information about this author
Nikhil Gawas
No information about this author
et al.
Natural Product Research,
Journal Year:
2024,
Volume and Issue:
unknown, P. 1 - 9
Published: Dec. 26, 2024
Diabetes
mellitus
is
a
rising
global
health
issue,
necessitating
effective
and
affordable
treatments.
This
study
aimed
to
develop
marker-based
quantification
methods
for
Diospyros
montana
Roxb
using
DoE
approach
conduct
in-silico
anti-diabetic
screening
of
its
phytoconstituents.
Methanolic
extracts
the
plant
underwent
fractionation,
with
chloroform
fraction
used
simultaneous
HPLC
Plumbagin
Juglone.
The
in-vitro
effects
were
evaluated
through
alpha-amylase
alpha-glucosidase
inhibition
assays.
Cytoscape
3.7.2
was
construct
networks
linking
phytoconstituents
Type-2
diabetes
targets
pathways,
while
docking
studies
involved
proteins
1SO2,
3H1V,
5DXU.
A
validated
method
quantified
(Rt:
4.618)
Juglone
3.998).
showed
significant
enzyme
IC50
values
36.775
33.124.
Gene
network
analysis
highlighted
8-hydroxyisodiospyrin,
revealed
Astragalin's
strong
binding
3H1V
(score:
−10.537).
underscores
potential
in
management,
warranting
further
research.
Language: Английский