A STABILITY INDICATING UV SPECROPHOTOMETRIC METHOD FOR DETERMINATION OF METOCLOPRAMIDE HYRDROCHLORIDE

A stability indicating method has been developed for specific determination of Metoclopramide HCl in bulk by UV spectrophotometry in presence of its degradation products. The method is simple, accurate, precise, and robust. Linearity range for the method is 10-50µg/ml at detection wavelength of 272 nm. The LOD and LOQ values were found to be 3.26µg/ml and 9.89µg/ml respectively

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF PIPERAQUINE PHOSPHATE AND DIHYDROARTEMISININ IN BULK

High Performance Liquid Chromatography (HPLC) methods are described for determination of drugs as a single or in combination in bulk or pharmaceutical formulation. The objective of the present study was to develop and validate novel, accurate, sensitive, precise, rapid and isocratic reverse Phase HPLC (RP-HPLC) method for the simultaneous determination of Piperaquine phosphate and Dihydroartemisinin in bulk because no method is available for simultaneous estimation of these drugs. The separation was achieved on GRACESMART RP-18 column (250 mm × 4.6 mm, 5μm) with mobile phase consisting of 10 mM Ammonium acetate (pH4.6, adjusted with Acetic acid): Methanol (15:85 % v/v) at a flow rate of 1.2 ml/min. UV detection at 220 nm. PQP and DHA obeyed linearity in the concentration range of 5-25 μg/ml (r2 = 0.9993) and 5-25 μg/ml (r2 = 0.9987) respectively. The asymmetric factors were found to be 1.17 for PQP and 1.2 for DHA. The developed method was validated as per ICH guidelines fulfill all the acceptance criteria and can be use for routine analysis

Paul Trap Mass Spectometer Developed in the Mass Spectometry Laboratory

The motivation of this technical report is to describe the design and provide fabrication details of the Paul trap mass spectrometer that has been built in our laboratory. This technical report gives both the theory of ion trapping in Paul trap mass spectrometers and the technical specifications of mechanical assembly, vacuum chamber and other electronic subsystems associated with our laboratory’s Paul trap mass spectrometer. Section 2 gives the theory of the ion trap mass spectrometry including development of equations of ion motion and the conditions required for the ions to have stable trajectories inside the trap. Section 3 provides the technical specifications of our trap electrodes, electronic subsystems including constant current source, gating power supply, extraction power supply, high voltage dc power supply, RF signal generator as well as the vacuum system and graphical user interface are presented. Section 4 presents a few mass spectra to demonstrate the performance our mass spectrometer. Appendix 1 gives the detailed orcad layouts of all the electronic circuits associated with the Paul trap mass spectrometer and the technical data related to the National Instruments data acquisition device PCI-MIO-16-E-1 is given in Appendix 2. At the end of the report a few important and pertinent references are provided

Development and validation of RP – HPLC method for quantitation of luliconazole in bulk and formulation

A new simple, specific, precise & validated Analytical Method has been developed for the determination of Luliconazole in bulk and pharmaceutical formulation. The separation was achieved on a C18 ODS (250×4.6 mm,5µm) or using mobile phase consisting of methanol: water (85:15) at a flow rate of 1.0 ml/min. Detection was carried out at 296nm. The retention time of Luliconazole was found to be 4.2min. the calibration curve found linear between range of 20-60 µg/ml with a regression coefficient of 0. 9998. The percentage recovery of Luliconazole was found to be in the range of 90-110%. The method was validated in accordance with International Conference on Harmonization. LOD & LOQ for Luliconazole were found to be 0.24μg & 0.748μg/ml respectively. Present method is simple, precise and can be used in routine analysis of Luliconazole in bulk and pharmaceutical lotion

Is there a hydrogen bond radius? Evidence from microwave spectroscopy, neutron scattering and x-ray diffraction results

Intermolecular distances in D-H…A hydrogen bonded systems have usually been interpreted in terms of the van der Waals radii of D and A. In this work, X-ray and neutron diffraction data from the Cambridge Crystal Structure Database (CSD) and the electrostatic potential of A, have been used to define hydrogen bond radii for OH, NH and CH groups. For OH, X-ray and neutron diffraction both give comparable results, validating the X-ray data for defining a hydrogen bond radius. The hydrogen bond radii determined for C≡CH and OH groups from CSD analysis are comparable to those determined from the gas phase rotational spectroscopic data for HCCH and H2O complexes. For NH as a proton donor, gas phase structural data are scarce and a hydrogen bond radius has been determined by using X-ray diffraction data only. For the CH group, the histogram of hydrogen bond distances shows a peak recognizable as a hydrogen bond only if it is acidic such as CCl3H, OCH (aldehydic) or CCH (acetylenic). The hydrogen bond radii for OH, NH and acidic CH groups are 0.60 ± 0.15, 0.76 ± 0.15 and 1.10 ± 0.20 Å, respectively. For C-CH3 and CH2CH3, though a peak in the histogram of distances is not found, the distribution of hydrogen bond angles unambiguously shows that the preferred geometry is linear. It appears that a CH group without any electronegative substituents could have a radius larger than 1.2 Å when involved in hydrogen bonding

Paul Trap Mass Spectometer Developed in the Mass Spectometry Laboratory

The motivation of this technical report is to describe the design and provide fabrication details of the Paul trap mass spectrometer that has been built in our laboratory. This technical report gives both the theory of ion trapping in Paul trap mass spectrometers and the technical specifications of mechanical assembly, vacuum chamber and other electronic subsystems associated with our laboratory’s Paul trap mass spectrometer. Section 2 gives the theory of the ion trap mass spectrometry including development of equations of ion motion and the conditions required for the ions to have stable trajectories inside the trap. Section 3 provides the technical specifications of our trap electrodes, electronic subsystems including constant current source, gating power supply, extraction power supply, high voltage dc power supply, RF signal generator as well as the vacuum system and graphical user interface are presented. Section 4 presents a few mass spectra to demonstrate the performance our mass spectrometer. Appendix 1 gives the detailed orcad layouts of all the electronic circuits associated with the Paul trap mass spectrometer and the technical data related to the National Instruments data acquisition device PCI-MIO-16-E-1 is given in Appendix 2. At the end of the report a few important and pertinent references are provided

A Convergent Continuous Multistep Process for the Preparation of C<inf>4</inf>-Oxime-Substituted Thiazoles

We report a strategy designed for the rapid and convergent assembly of C4-oxime substituted thiazoles. Our approach relied on 3-bromo-2-oxopropanal O-methyl oxime 7 as a key building block. A three-step sequence to 7 was designed, which for safety concerns, could only be operated in batch mode on limited scales (<< 100g). We describe herein how we addressed such a limitation, by designing a multistep continuous synthesis of this intermediate and further demonstrate the advantages of flow reactor configuration upon scaling up.Syngent