Development and Validation of Stability-Indicating Impurity Profiling Method for Azelastine Hydrochloride and Fluticasone Propionate in Nasal Spray Product Using HPLC with a UV/PDA Detector.

BACKGROUND: Azelastine HCl (AZ) and fluticasone propionate (FL) nasal spray drug product is commonly used in the treatment of allergic rhinitis worldwide. To date, the impurity profiling of this product has not been reported. OBJECTIVE: The present study aimed to develop and validate a novel RP-HPLC stability-indicating analytical method for the estimation of impurities from AZ and FL nasal spray drug product. METHODS: A mixture of octane sulfonic acid sodium salt and trifluroacetic acid is used as a mobile phase A. Acetonitrile is used as a mobile phase B. Good separation was achieved on Baker bond phenyl hexyl, 250 × 4.6, 5 µm column at 1 mL/min flow rate in gradient elution mode. The chromatograms were monitored at 239 nm. RESULTS: The LOD and LOQ were found to be 0.006 and 0.019 µg/mL for AZ and 0.010 and 0.030 µg/mL for FL, respectively. The correlation coefficient for all the known impurities and principal analytes was 0.999 from LOQ level to 150% of standard concentration. The recovery for all the known impurities was found to be between 90 and 110%. In the stress study, 15% degradation was observed in basic conditions and 8.7% in acidic conditions. No significant degradation was observed in thermal and oxidative conditions. CONCLUSION: An impurity profiling method for AZ and FL combination nasal spray product was successfully developed, validated, and demonstrated to be accurate, precise, specific, robust, and stability-indicating. The method can be routinely used for impurity testing of commercial batches in QC laboratories in the pharmaceutical industry. HIGHLIGHTS: No impurity study has been reported for this combination product until now.

Benefits of Soleris® over the Conventional Method for Enumeration of Microbial Load in Salacia Herbal Extract.

Stems and roots of Salacia genus plants have been used as a specific remedy for early-stage diabetes, and one of the four sulphonium sulphates, salacinol is the compound responsible for the anti-diabetic activity. Salacia is prone to microbial contamination and insect infestation; hence, methods to estimate the microbial load in such plants will enhance its nutritional value. This paper highlights the novel use of Soleris® to quantify microbes of all types, namely bacteria, yeasts, molds, and coliforms in herbal extracts. The microbial analysis results obtained with Soleris® test vial have been compared with the conventional method, and the results indicate that Soleris® is equally efficient as the conventional method and in fact displays several advantages over the traditional method. The Soleris® method is a real time monitoring system that is highly sensitive, user-friendly, and environmentally friendly since it generates very little biomedical waste and saves a large amount of time. The data presented here demonstrate that for highly contaminated samples, results are available within 24 h. For yeasts and molds, the Soleris® method produces results in 48 h, thus offering considerable time savings compared to other commonly used methods.

Design and development of a stable polyherbal formulation based on the results of compatibility studies.

INTRODUCTION: Ayurvedic and herbal medicinal products contain a combination of botanicals; each of these contains a number of chemical compounds that may give the anticipated activity in combination. Therefore, it is very important to analyze and evaluate the compatibility of various active constituents and markers from different medicinal plants for their possible chemical interactions with various excipients at different storage conditions during the development of a stable polyherbal formulation. OBJECTIVE: To study chemical stability of kalmegh (Andrographis paniculata) and kutki (Picrorhiza kurroa) extract for their active markers andrographolide, kutkoside and picroside-I and to develop stable polyherbal formulation based on the incompatibility studies. MATERIALS AND METHODS: The compatibility study was carried out on individual ethanolic extracts of these two plants along with the commonly used excipients in the ratio of 1:1 at 40 ± 2°C and 75 ± 5% relative humidity and at a refrigeration temperature of 5 ± 1°C for initial, 7-, 15- and 30-day intervals. The analysis was carried out using the validated reverse phase-high-performance liquid chromatography methods. A stable tablet dosage form was developed based on the results of these studies. RESULT: The study suggested that the active markers of kutki (kutkoside and picroside-I) were found to be degraded in the presence of the kalmegh extract. However, the active marker of the kalmegh extract (andrographolide) was found to be stable. Both the extracts showed excellent compatibility with all the excipients used in making this formulation. No significant decrease in the kutkoside and picroside-I content from the formulation was observed. CONCLUSION: By separate granulation process the exposure of both the extracts can be minimized thus avoiding the degradation of active markers.

Rapid microwave-assisted extraction and HPTLC-photodensitometric method for the quality assessment of Boerhaavia diffusa L.

A rapid and cost-effective method for the extraction of rotenoids in Boerhaavia diffusa L., based on the use of microwave-assisted extraction (MAE), is proposed. The conventional reflux, soxhlet, and maceration extraction methods were also conducted to validate the reliability of the new method. Under the optimized conditions, two rotenoids (boeravinone B and E) were extracted and quantified by HPTLC. The yield of boeravinone B and E achieved by MAE was 0.15 and 0.32% (w/w), respectively. The result showed that MAE-HPTLC is a simple, rapid, and solvent-sparing method for the extraction and quantitation of boeravinone B and E from B. diffusa L.