A chromatographic fingerprint is a comprehensive method that reveals the distinctive pattern of peaks across the chromatogram for a given sample. It is considered an effective strategy to assess the identity and quality of herbal materials, as well as for the control of the quality of their derived products. HPLC is the most employed technique for these purposes and it is used routinely for quality control in industry. Hence, its impact on the environment should not be neglected. This work provides a rational and generic procedure to qualitatively fingerprint complex matrices. Resource- and time-saving experimental designs were selected; an alternative safer organic solvent was tested and a time-saving and innovative response entitled the green chromatographic fingerprinting response was developed and employed. This procedure was applied in the development of chromatographic fingerprints for extracts of Bauhinia forficata and Casearia sylvestris. Moreover, the response proposed here can be combined with a complementary metric available in the literature to compare methods using different solvents. According to this, the chromatographic fingerprints developed here using ethanol as the organic solvent provided a performance better than that of reference methods in which more harmful acetonitrile or methanol were employed.
Pharmaceutical
cocrystals are mixed crystals that contain two or
more different molecular components. These crystals usually present
different characteristics from their precursor, an improvement in
the drug solubility being the most important property. This article
is the first to report a green synthesis of ibuprofen–nicotinamide
cocrystal in aqueous media. The use of safer solvents and in-line
monitoring are some of the green chemistry principles that should
be evaluated in environmentally correct synthesis. The Raman spectroscopy
as a PAT tool provided an effective in line method to monitor and
quantify the reaction. This is the first report of the cocrystal of
ibuprofen–nicotinamide obtained by slurry conversion. A total
conversion of the initial substrates into the cocrystal was obtained
in mild conditions. The use of chemometric tools and Raman spectroscopy
made it possible to monitor and understand the cocrystallization mechanism,
and the synthesis provided.
A considerable amount of chemical waste from liquid chromatography analysis is generated worldwide. Acetonitrile is the most employed solvent in liquid chromatography analyses since it exhibits favorable physicochemical properties for separation and detection, but it is an unwelcome solvent from an environmental point of view. Acetone might be a much greener alternative to replace acetonitrile in reversed-phase liquid chromatography, since both share similar physicochemical properties, but its applicability with ultraviolet absorbance-based detectors is limited. In this work, a reference method using acetonitrile and high-performance liquid chromatography coupled to an ultraviolet photodiode array detector coupled to a corona charged aerosol detector system was developed to fingerprint a complex sample. The possibility of effectively substituting acetonitrile with acetone was investigated. Design of experiments was adopted to maximize the number of peaks acquired in both fingerprint developments. The methods with acetonitrile or acetone were successfully optimized and proved to be statistically similar when only the number of peaks or peak capacity was taken into consideration. However, the superiority of the latter was evidenced when parameters of separation and those related to greenness were heuristically combined. A green, comprehensive, time- and resource-saving approach is presented here, which is generic and applicable to other complex matrices. Furthermore, it is in line with environmental legislation and analytical trends.
Pharmaceutical cocrystals
have emerged over the past several decades
as an alternative path for synthesizing stable and/or improved crystalline
forms of active pharmaceutical ingredients. In this contribution,
we developed a reproducible cocrystallization path for the supramolecular
synthesis of four new pharmaceutical cocrystal forms of fluconazole
(FLZ), an antifungal multifunctional drug: fluconazole–fumaric
acid monohydrate (1:1:1), fluconazole–malic acid (1:1), fluconazole–dipicolinic
acid (1:1), and fluconazole–adipic acid (1:1). All the new
cocrystals were characterized by powder/single-crystal X-ray diffraction,
Raman, Fourier transform infrared spectroscopy, differential scanning
calorimetry/thermogravimetric analysis, and hot-stage polarized optical
microscopy, and their water solubility was determined. Structurally,
although the coformers were different, the same strong O–H···N
hydrogen bond between the FLZ molecule and the coformers was observed.
The aqueous solubility studies revealed that all the cocrystals were
found to exhibit improved aqueous solubility when compared to the
commercialized FLZ polymorph.
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