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Xiaomi Redmi 7 3GB. Coolpad Note 8. Available on 2 stores. Vivo Y91i 32GB. Xiaomi Redmi 6 64GB. Samsung Galaxy J4 Plus. Vivo Y91i 16GB. Nokia 3. Moto E6s. Vivo Y The recrystallization tests that were performed indicated that higher temperatures showed a distinct increase in the rate of recrystallization and that each technique provided similar results within experimental error. It is also important to note that each technique gave similar spectra where applicable , which provides supporting evidence that the data is meaningful. Overall, the conclusions of this research were that low-frequency predictions of crystallinity are at least as accurate as the predictions made using mid-frequency Raman techniques.
It is arguable that low-frequency Raman is better because of the presence of stronger spectral features and because they are intrinsically linked with crystallinity. The ranges of interest were indicated to be 5— cm -1 and — cm -1 regions.
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Samples of indomethacin were milled using a cryogenic mill to avoid mechanical heating of the sample, with full amorphous samples being obtained after 25 min of milling. Methods used in this study include Raman spectroscopy, isothermal differential scanning calorimetry DSC , and X-ray diffractometry as well as the milling technique.
The results of this research did in fact show that low-frequency Raman spectroscopy is a very sensitive technique for identifying very small amounts of crystallinity within mostly amorphous samples. This paper particularly noted the benefit of low acquisition times associated with low-frequency Raman spectroscopy compared with the other techniques used.
Low-frequency Raman spectroscopy was also used to monitor two polymorphic forms of caffeine after grinding and pressurization of the samples Pressurization was performed hydrostatically using a gasketed membrane diamond anvil cell MDAC , while ball milling was used as the method of grinding the sample. Analysis methods used were low-frequency Raman and X-ray diffraction.
Low-frequency Raman spectra revealed that, upon slight pressurization, caffeine form I transforms into a metastable state slightly different from that of form II and that a disordered amorphous state is achieved in both forms when pressurized above 2 GPa. In contrast, it is concluded that grinding results in the transformation of each form into the other with precise grinding times, thus also generating an intermediate form, which was found to only be observable using low-frequency Raman spectroscopy.
Larkin and colleagues 41 used low-frequency Raman in conjunction with other techniques to characterize several different APIs and their various forms. The APIs studied include carbamazepine, apixaban diacid co-crystals, theophylline, and caffeine and were prepared in various ways that are not detailed here. During this research, low-frequency Raman spectroscopy played an important role in understanding the structures while in their various forms. However, more importantly, low-frequency Raman spectroscopy produced information-rich regions below cm -1 for each of the crystalline samples and noticeably broad features when the APIs were in solution.
Wang and colleagues 42 investigated the applicability of low-frequency Raman spectroscopy in the analysis of respirable dosage forms of various pharmaceuticals. The analyzed pharmaceuticals were involved in the treatment of asthma or chronic obstructive pulmonary disease COPD and include salmeterol xinafoate, formoterol fumarate, glycopyrronium bromide, fluticasone propionate, mometasone furoate, and salbutamol sulfate. Various formulations of amino acid excipients were also analyzed in this study.
Results indicated that the use of low-frequency Raman analysis was beneficial because of the large features found in the region and allowed for reliable identification of each of the dosage forms. Not only this, it also allowed unambiguous identification of two similar bronchodilators, albuterol Ventolin and salbutamol Airomir. Heyler and colleagues 43 collected both the low-frequency and fingerprint region of Raman spectra from several polymorphs of carbamazepine, an anticonvulsant and mood stabilizer. This study found that the different polymorphs of this API could be distinguished effectively using these two regions.
Similarly, Al-Dulaimi and colleagues 44 demonstrated that polymorphic forms of paracetamol, flufenamic acid, and imipramine hydrochloride could be screened using low-frequency Raman and only milligram quantities of each drug. In this study, paracetamol and flufenamic acid were used as the model compounds for comparison with a previously unstudied system imipramine hydrochloride. Features within the low-frequency Raman regions of spectra were shown to be significantly different between forms of each drug. Therefore this study also indicated that the polymorphs were highly distinguishable using the technique.