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Abstract  

The physico-chemical properties and polymorphism of a new active pharmaceutical ingredient entity has been analyzed and the gain of knowledge during the chemical development of the substance is described. Initial crystallization revealed an anhydrous crystal form with good crystallinity and a single, sharp DSC melting peak at 171C and a straightforward development of this crystal form seemed possible. However, during polymorphism screening, new crystalline forms were detected that were often analyzed as mixtures of crystal forms. The process of characterization and identification of the different crystalline forms and its thermodynamical relationship has been supported by a combination of experimental and computational work including determination of the three-dimensional structures of the crystal forms. The crystal structure of one polymorphic form was solved by single crystal X-ray structure analysis. Unfortunately, Mod B resisted in formation of suitable single crystals, but its structure could be solved by high resolution powder diffraction data analysis using synchrotron radiation. Calculation of the theoretical X-ray powder diffraction pattern from three dimensional crystal coordinates allowed an unambiguous identification of the different crystalline forms. Two polymorphic crystal forms of the API-CG3, named Mod A and Mod B, are enantiotropic whereas Mod B is the most stable polymorph at room temperature up to about 50C and Mod A at temperatures above 50C. The mechanism of the solid-solid transition can be explained by analyzing the molecular packing information gained from the single crystal structures. A third crystalline form with the highest melting peak turned out to be not a polymorphic or pseudopolymorphic crystal modification of our API-CG3 but a chemically different substance.

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Enantioresolution of three active pharmaceutical ingredients (APIs), namely, atenolol, betaxolol, and orciprenaline, marketed as racemic mixture, has been achieved in a direct mode using (S)-glutamic acid as chiral additive in thin-layer chromatography. Two different approaches were adopted: (1) (S)-glutamic acid was mixed in the silica gel slurry for making thin-layer plates, or (2) it was added in the mobile phase and plain plates without any chiral additive were used. Both (1) and (2) were capable of separating enantiomers of all the three racemates, but different combinations and proportions of solvents were found successful in the two cases. Good resolution was achieved in both cases, and the results are compared for these two sets of studies among themselves and with other literature reports. Iodine was used to locate the spots of the corresponding enantiomers. The detection limits for each enantiomer were found in the range of 1.4–1.9 μg (per spot).

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Abstract  

Amorphization is nowadays a method that is frequently applied in the pharmaceutical industry. The primary aim of this study is to achieve the amorphization of clopidogrel hydrogen sulphate as an active pharmaceutical ingredient (API) with various solvents and to choose the most suitable one. A secondary aim was to determine the glass-transition temperature (T g) of this API and to classify it as a good or poor glass former. To investigate the amorphous form, differential scanning calorimetry, X-ray powder diffraction, and FT-IR analysis were applied. The melting point (T m) was 177.4 °C (450.6 K), and T g was determined to be 88.9 °C (362.1 K). The quotient T g/T m was 0.80, and this API was therefore classified as a good glass former.

Open access

This work represents the validation of a stability-indicating thin-layer chromatographic technique for the simultaneous estimation of metolazone (METO) and spironolactone (SPIRO) from marketed formulation (tablets). Thin-layer chromatography was performed using precoated silica gel plate 60 F254 using ethyl acetate—chloroform—GAA (5:5:0.1 v/v) as the mobile phase for the separation of METO and SPIRO. The stability study forms an integral part of the formulation development process, and its use is also encouraged by various guidelines. Stress study was performed on active pharmaceutical ingredients (APIs) as well as on formulation for establishing a stability-indicating thin-layer chromatographic method for both drugs. The APIs were subjected to change under various environmental conditions such as pH, temperature, oxidation, etc. to determine their effect on the stability of drugs. The developed method was able to resolve drugs and their degradation products formed under the aforementioned conditions. The wavelength selected for quantitation was 238 nm. The method was validated as per the International Conference on Harmonization (ICH) guidelines and found to be linear in the range of 50–300 ng spot−1 for METO and 200–1200 ng spot−1 for SPIRO. The relative standard deviation (% RSD) values of the precision study were <2% which indicated that the developed method was precise; recovery was found to be 99.02–100.58% and 99.26–100.17% for METO and SPIRO, respectively. It could be concluded from the stability study that METO was prone to acidic hydrolysis and photolysis while SPIRO was prone to alkaline degradation.

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-performance liquid chromatography with diode array detection (HPLC–DAD) method for simultaneous determination of related substances in TBI-166 active pharmaceutical ingredient (API) was established and fully validated. Ten kinds of potential impurities of TBI-166 API

Open access

simultaneous determination and quantification of TRM and XIP in active pharmaceutical ingredients and co-formulated pharmaceutical dosage forms. High accuracies and precisions results were obtained. The validated method had lower solvent consumption, replaced

Open access

environment 4 Conclusion In the proposed study, a green HPLC method was developed and validated for the simultaneous determination and quantification of TRM and XIP in active pharmaceutical ingredients and co-formulated pharmaceutical dosage forms. High

Open access

with the big round bottom flask. Active pharmaceutical ingredients are synthesized in manufacturing plants and then shipped to other sites to be converted into a form that can be given to patients, such as tablets, drug solutions, or suspensions

Open access

achievements of synthetic organic chemistry have been illustrated by the total syntheses of complex natural products or valuable molecules such as active pharmaceutical ingredients (APIs) and agrochemicals from simple natural sources. These syntheses were

Open access

typical, and control at parts per million (ppm) levels is not uncommon [ 8 ]. Control of residual solvents, inorganics, and metals as well as polymorph/form control of the final active pharmaceutical ingredient (API) must also be established. Commercial

Open access