ABSTRACT
Objective: Aim of the present research work was to develop a sensitive, rapid and accurate, stability-indicating RP-UPLC method for the simultaneous estimation of tezacaftor and ivacaftor in formulations. Methods: The chromatographic separation of the mixture of tezacaftor and ivacaftor was attained in isocratic method utilizing a mobile phase of 0.1 % orthophosphoric acid and acetonitrile in the proportion of 50:50%v/v utilizing a HSS C18 column which has dimensions of 100×2.1 mm, 1.7 m particle size and the flow rate of 0.3 ml/min. The detection system was monitored at 292 nm wavelength maximum with 1.5 ml injection volume. The present method was validated as per the guidelines given by the ICH for specificity, accuracy, sensitivity, linearity and precision. Results: The retaining time for tezacaftor and ivacaftor were achieved at 1.071 min and 0.530 min, respectively. Tezacaftor, ivacaftor and their combined drug formulation were exposed to thermal, acidic, oxidative, photolytic, and alkaline conditions. The developed method was highly sensitive, rapid, precise and accurate than the earlier reported methods. The total run time was decreased to 2.0 min; hence, the technique was more precise and economical. Stability studies directed for the suitability of the technique for degradation studies of tezacaftor and ivacaftor. Conclusion: The projected method can be utilized for routine analysis in the quality control department in pharmaceutical trades.
ABSTRACT
The objective of the work is to develop and validate a new reverse phased ultra-performance chromatography method and its stability studies for the simultaneous estimation of alogliptin and pioglitazone in bulk and tablet dosage form. The column of the method was BEH C18 (2.1× 50 mm, 1.7 µ) used as a stationary phase and the mobile phase was 45:55 v/v of phosphate buffer (pH 3) and methanol, respectively. The injection volume was 2 µl and flow rate was maintained at 0.3 ml/minute. The wavelength was 280 nm and the runtime was 3 minutes. The retention time of alogliptin was 0.4 minutes and pioglitazone was 0.529 minutes. The Linearity of the alogliptin was 6.25–37.5 µg/ml and pioglitazone was 15–90 µg/ml. The newly developed method could be used for the routine analysis of pure drug and its formulations in accordance with the ICH Q2 (R1) guidelines.
ABSTRACT
OBJECTIVE: To develop an intergrated urinary metabonomic strategy based on RP-UPLC-MS and HILIC-UPLC-MS method and to investigated the mechanism of osteoporosis and the prevention effect of glucocorticoid osteoporosis of Gushudan. METHODS: The RP-UPLC-MS and HILIC-UPLC-MS method were developed for rat urine metabolite profiling study among control group, model group and Gushudan treatment group. Principal component analysis (PCA) were used to find the biomarkers, further more, to explore the mechanism of the prevention effect on glucocorticoid osteoporosis of Gushudan. RESULTS: In the mode of RP-UPLC-MS, low polarity metabolites like phenylacetylglycine, N2-succinic acid-L-ornithine were found while relatively high polarity metabolites like betaine, hypoxanthine were found in the mode of HILIC-UPLC-MS. And twenty-two potential biomarkers have been totaly found in the urine of glucocorticoid osteoporosis, primiarily related to amino acid metabolism, energy metabolism, lipid metabolism, intestinal flora metabolism and kidney damage. Gushudan has intervention effects on rats with osteoprosis via the regulation of multiplemetabolic pathways. CONCLUSION: The combination of RP-UPLC-MS and HILIC-UPLC-MS method can give a more comprehensive profiling of endogenous metabolites and it also indicates metabonomic strategy has become a powerful tool to evaluate the overall efficacy of traditional Chinese medicine (TCM) and to calrify the mechanism of TCM.
ABSTRACT
A stability indicating RP-UPLC method was developed and validated for the simultaneous determination of Thiocolchicoside (TCC) and Aceclofenac (ACF) in tablet dosage form. The chromatographic separation was carried out by Thermo Scientific UPLC Instrument, Accela 1250 Pump, auto sampler with PDA detector, using column Thermo Scientific hypersil gold C18, (50 x 2.1mm) particle size 1.9μm using 5% ammonium acetate buffer and methanol in the ratio of 40:60, pH was adjusted to 5 with ortho phosphoric acid as mobile phase at a flow rate of 250 μl/min with the detection at 276nm. The run times of the TCC and ACF were about 0.697 and 1.125 minutes, respectively. The detector response is linear from 4.8 μg/ml to 7.2 μg/ml and 63.8 μg/ml to 96 μg/ml concentrations for TCC and ACF respectively. The linear regression equation was found to be y = 20620x-677.68 (r2 = 0.9996) for TCC and y= 50931x-319.3 (r2 = 0.9997) for ACF. The detection limit and quantification limit was 0.076μg and 0.23μg for TCC and 0.27μg and 0.71μg for ACF. The percentage of assay of TCC and ACF were about 99.50% and 99.96% respectively. The stability indicating capability was established by forced degradation experiments. The method was satisfactorily validated as per the ICH guidelines.
ABSTRACT
A stability indicating RP-UPLC method was developed and validated for the simultaneous determination of Thiocolchicoside (TCC) and Aceclofenac (ACF) in tablet dosage form. The chromatographic separation was carried out by Thermo Scientific UPLC Instrument, Accela 1250 Pump, auto sampler with PDA detector, using column Thermo Scientific hypersil gold C18, (50 x 2.1mm) particle size 1.9μm using 5% ammonium acetate buffer and methanol in the ratio of 40:60, pH was adjusted to 5 with ortho phosphoric acid as mobile phase at a flow rate of 250 μl/min with the detection at 276nm. The run times of the TCC and ACF were about 0.697 and 1.125 minutes, respectively. The detector response is linear from 4.8 μg/ml to 7.2 μg/ml and 63.8 μg/ml to 96 μg/ml concentrations for TCC and ACF respectively. The linear regression equation was found to be y = 20620x-677.68 (r2 = 0.9996) for TCC and y= 50931x-319.3 (r2 = 0.9997) for ACF. The detection limit and quantification limit was 0.076μg and 0.23μg for TCC and 0.27μg and 0.71μg for ACF. The percentage of assay of TCC and ACF were about 99.50% and 99.96% respectively. The stability indicating capability was established by forced degradation experiments. The method was satisfactorily validated as per the ICH guidelines.