Chapter-IV

Conclusion

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4.1Moxifloxacin

The drug's less hydrated, anhydrate, and amorphous forms modified the crystal lattice.
Loss of 1-mole of channel water from MHM leads to the formation of a stable semi-
crystalline phase distinct from initial hydrates. It does not instantly come to its initial
state/phase under relevant conditions. The variations in the X-ray diffraction pattern
from the initial MHM indicate the creation of a new phase with dehydration.

Dehydrated drug substance also shows differences in the thermal transitions than that
of pure monohydrate form. These transitions show sharper with more change in
enthalpy endothermic peaks due to the loss of a mole of water from the crystal lattice.
This rearrangement in the crystal lattice affects the physical strength of the dehydrated
crystal form due to fractures. It produces crystals with slightly larger particle sizes due to
amorphisation, leading to gelatinisation. This increase in particle size is evident from
particle size distribution data.

Similarly, compaction during the manufacturing process plays a vital role and can impact
the physicochemical properties of the final drug product on its dissolution and bio
performance. An increase in particle size due to compaction decreases the specific
surface area and reduces the degree of crystallinity. Based on the outcome of dissolution
and solubility profile, particle size plays a vital role as its increase lowers the dissolution
rate

Understanding this physical consequence of the change in particle size during

4.2 Compound D Method

The developed RP-HPLC method was found to be simple, specific, sensitive, accurate,
precise and stability indicating. The %Recovery and %RSD value indicating the

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reproducibility and accuracy of the proposed method. The method intended to be
specific as there is no interference observed with respect to blank, indicating the
developed method is ready for the future new molecule of Sulfonamide- Anthranilate
derivative.

4.3 Baricitinib Impurity Method

The available literature revealed that limited methods available for Baricitinib along with
its few impurities and degradants. But no any single method available for the
determination of Baricitinib, above cited all impurities with its degradants. A new
gradient HPLC method has been developed and validated for the analysis of Baricitinib,
all impurities and degradation products. The method has been validated for the
specificity, linearity, accuracy,precision and robustness. The method is capable to
quantify all impurities in the presence of main drug and other unspecified impurities. The
degradation study proves that formed unknown impurities can be well resolved without
any interference. The method is linear in the range of LOQ to 250 % for all impurities
with correlation coefficient greater than 0.99. The method is accurate and precise. Also
as the method is validated according to ICH guideces it could be used for the analysis of
related substances in the bulk drug and formulation in quality control laboratory and
pharmaceutical industries

4.4 Molnupiravir Impurity Method

The existing literature denotes that few methods obtainable for Molnupiravir with its
some impurity and degradants. But no any method is existing for determination of above
listed impurities of Molnupiravir with its degradants. A new LC-MS compatible gradient
HPLC method has been developed and validated for the analysis of Molnupiravir, its all
impurities and degradation products. The method has been validated for the specificity,
linearity, accuracy, precision, robustness and solution stability. The method is able to
quantify all impurities in the presence of main drug and other unspecified impurities. The
degradation study proves that formed unknown impurities can be well resolved without
any interference. The method is linear in the range of LOQ to 250 % for all impurities

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with correlation coefficient greater than 0.99. The method is accurate and precise. Also
as the method is validated according to ICH guidences it could be used for the analysis of
related substances in the bulk drug and formulation in quality control laboratory and
pharmaceutical industry.

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