Fast and simple gas chromatographic method for simultaneous estimation of camphor, menthol and methyl salicylate in analgesic ointment: application in stability study

A simple, rapid and sensitive gas chromatographic (GC) method with flame ionization detector (FID) has been developed and validated for simultaneous estimation of camphor, menthol and methyl salicylate (MS). Camphor, menthol and MS were separated at about 2.753, 3.206 and 3.995 min respectively on a capillary column with helium (3.3 ml/min) as carrier gas within 11 min run time. Noninterference of any peak with the peaks of interest confirms the selectivity of method. Derived quantitation limits (QL) were 0.847, 0.684 and 6.507 μg/ml for camphor, menthol and MS respectively. The linear relationship ( R2 > 0.999) between analyte concentration vs detector response was established within a range of QL to 150% of label claim concentration for each analyte. Recovery of each analyte at 50, 100 and 150% of label claim concentration levels were obtained within 99.67–101.53% establishing high accuracy of the method. The method showed acceptable precision with low relative standard deviation or RSD (0.24–1.03%) between percent recoveries for each analyte. RSD for intermediate precision (inter day analysis, analyst variation) was less than 1%. The validated method was successfully applied for quantitative determination of camphor, menthol and MS in stability samples of an analgesic ointment produced by IKOP Sdn. Bhd., Malaysia

Fusion between contemporary medicine (paracetamol) and prophetic medicine (honey) as pharmaceutical suspension

Commercial paracetamol (PCM) suspension is formulated with high amount of sugar and more than 7 excipients to mask the bitter taste of PCM and to achieve stable pharmaceutical suspension for an acceptable shelf-life. This over-the counter pharmaceutical is rampantly used to alleviate minor ailments and fever especially in infants and children but concern over its high sugar sweeteners content during repeated and prolonged treatment is worrying (e.g. dental caries). As such, this study aims to explore alternative PCM formulation by fusioning the PCM into honey alone without other excipients. Two types of honey have been tested, namely ‘Khaula’ and ‘Tualang’ which differ in viscosity and colour. Different processing variables had been tested as well including type of mixers, temperature and flow rate. The formulation were characterised for their particle size, stability and compatibility and the results were compared with commercial PCM suspension. PCM suspension prepared using highly viscous honey (Khaula) was found to be stable compared to the commercial PCM in contrast to PCM-Tualang suspension. Compatibility study based on Fourier-Transform Infra-Red (FTIR) showed similar spectra for all PCM-honey as compared to commercial PCM. Particle size of PCM-Khaula was larger than PCM-Tualang due to different processing method and equipments employed. To conclude, honey appeared to be compatible with PCM and produced stable suspension without the need for other excipients. The fusion of honey is also expected to confer its wholesome benefits to the pharmaceuticals and may improve the treatment of relevant indication

Development and characterization of topical analgesic ointment - from laboratory to production scale

The purpose of this study was to scale up an ointment formulation containing 25% w/w methyl salicylate, developed via 300-g laboratory batches to 45-kg batch sizes in a homogenize mixer. Method: The ointment was manufactured by fusion method in a homogenous mixer. Characterization was conducted for assay of ingredients by a validated GC-FID method, physicochemical properties and microbial limit test. Further, optimized formulation was scaled up at large scale. Result: The desired analgesic ointments were developed and evaluated which contains petrolatum base (30%), Beeswax 1540 (20%) , methyl salicylate (10%), Menthol crystal (5 %),Camphor powder (5 %). The drug content were within specification. The stable formulation was observed during laboratory scale as well as at production scale. Successful scale up for 45kg batches were carried out. Conclusion: A topical analgesic ointment was developed and successfully scaled up that can be commercialized after meeting relevant regulatory requirements