scholarly journals ISOLATION AND CHARACTERISATION OF RAPAMYCIN, TEMSIROLIMUS REGIO ISOMER (MONOESTER) AND TEMSIROLIMUS DIESTER IN TEMSIROLIMUS DRUG

Author(s):  
Gorla S. Reddy ◽  
Chava V. N. Rao

Objective: Separation and identification of the process impurities in the manufacture of temsirolimus drug viz., rapamycin, temsirolimus regioisomer (monoester) (TS monoester), and temsirolimus diester (TS diester). Methods: During the process development of temsirolimus (TS), three process impurities-rapamycin, temsirolimus regioisomer (monoester) and temsirolimus diester-were detected by high-performance liquid chromatography (HPLC). Impurities were isolated by medium pressure liquid Chromatography (MPLC) and characterized by ESI-MS/MS, 1H NMR, FT-IR spectral data. Results: These impurities are characterised with the help of ESI MS/MS, 1H NMR, and FT-IR data. The impurities are identified and characterised as the process impurities. One of them is the starting material i.e. rapamycin and the other two are formed during the manufacture of the drug. This method offers advantages over using photodiode-array UV detection (LC-PDA) for the determination of peak purity, viz. components with similar UV spectra can be distinguished. Conclusion: The structures of these impurities were characterized as rapamycin, TS Monoester, and TS Diester. Out of these process impurities, rapamycin has been previously identified while the other two are previously unreported.

1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.


Insects ◽  
2021 ◽  
Vol 12 (4) ◽  
pp. 340
Author(s):  
Kitherian Sahayaraj ◽  
Balakrishnan Saranya ◽  
Samy Sayed ◽  
Loko Yêyinou Laura Estelle ◽  
Koilraj Madasamy

The foam produced by nymphs of Poophilus costalis on eleven different host plants belonging to eight families on St. Xavier’s College campus in India was studied over five months. The chemical composition and antimicrobial activity of these biofoams were investigated. The results revealed that P. costalis preferred Theporsia purpurea and Mimosa pudica for laying their eggs and producing foam, over the other tested plants. P. costalis produce their foam on either nodes or internodes on monocotyledons (30%) (p < 0.05), whereas on dicotyledons, they produce more foam on the stems (63.8%) than on the leaves (6.2%) (p < 0.01). The number of nymphs in each piece of foam from P. costalis varied from 1 to 3 (mean = 1.8 per plant). They produced their foam (5.7 to 45.2 cm) from the ground level on a plant. The length and breadth of a piece of foam ranged from 1.0 to 3.9 cm and 0.6 to 4.7 cm, respectively. The foam tended to be cooler than the environment. Qualitative profiling showed that the foam consists of carbohydrates, including maltose; trypsin; amino acids; protease. The foam was also analyzed using a spectrophotometer, Fourier transform infrared spectroscopy (FT-IR), gas chromatography–mass spectroscopy (GC-MS), and high-performance liquid chromatography (HPLC). The antimicrobial activity of the biofoam was the greatest against Staphylococcus aureus, the growth of which was reduced by 55.9 ± 3.9%, suggesting that the foam could be used as an antimicrobial product. However, no activities were observed against Fusarium oxysporum and Candida albicans.


1992 ◽  
Vol 605 (2) ◽  
pp. 221-225 ◽  
Author(s):  
Marcello Previti ◽  
Francesco Dotta ◽  
Giuseppe Mario Pontieri ◽  
Umberto Di Mario ◽  
Luisa Lenti

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