scholarly journals Stability of extemporaneously compounded amiloride nasal spray

2020 ◽  
Author(s):  
Venkata Yellepeddi ◽  
Casey Sayre ◽  
Anna Burrows ◽  
Kevin Watt ◽  
Simon Davies ◽  
...  
Keyword(s):  
United States ◽  
Nasal Spray ◽  
Room Temperature ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Indicating ◽  
Spray Solution ◽  
Microbiological Stability ◽  
The Stability ◽  
Amiloride Hydrochloride

AbstractAnxiety disorders (AD) are the most common mental illnesses affecting an estimated 40 million adults in the United States. Amiloride, a diuretic agent, has shown efficacy in treating AD in preclinical models by inhibiting the acid-sensing ion channels (ASIC). By delivering amiloride via nasal route, rapid onset of action can be achieved due to direct “nose-to-brain” access. Therefore, this study reports the formulation, physical, chemical, and microbiological stability of an extemporaneously prepared amiloride 2 mg/mL nasal spray. The amiloride nasal spray was prepared by adding 100 mg of amiloride hydrochloride to 50 mL of sterile water for injection in a sterile reagent bottle. A stability-indicating high-performance liquid chromatography (HPLC) method was developed and validated. Forced-degradation studies were performed to confirm the ability of the HPLC method to identify the degradation products from amiloride distinctively. The physical stability of the amiloride nasal spray was assessed by pH, clarity, and viscosity assessments. For chemical stability studies, samples of nasal sprays stored at room temperature were collected at time-points 0, 3 hr., 24 hr., and 7 days and were assayed in triplicate using the stability-indicating HPLC method. Microbiological stability of the nasal spray solution was evaluated for up to 7 days based on the sterility test outlined in United States Pharmacopoeia (USP) chapter 71. The stability-indicting HPLC method identified the degradation products of amiloride without interference from amiloride. All tested solutions retained over 90% of the initial amiloride concentration for the 7-day study period. There were no changes in color, pH, and viscosity in any sample. The nasal spray solutions were sterile for up to 7 days in all samples tested. An extemporaneously prepared nasal spray solution of amiloride hydrochloride (2 mg/mL) was physically, chemically, and microbiologically stable for 7 days when stored at room temperature.

Development and Validation of a Stability Indicating RP-HPLC Method for Hydrocortisone Acetate Active Ingredient, Propyl Parahydroxybenzoate and Methyl Parahydroxybenzoate Preservatives, Butylhydroxyanisole Antioxidant, and Their Degradation Products in a Rectal Gel Formulation

2015 ◽  
Vol 98 (1) ◽  
pp. 27-34 ◽  
Author(s):  
Magda Ascaso ◽  
Pilar Pérez-Lozano ◽  
Mireia García ◽  
Encarna García-Montoya ◽  
Montse Miñarro ◽  
...  
Keyword(s):  
Active Ingredient ◽  
Active Substance ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Hydrocortisone Acetate ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
The Stability

Abstract A stability indicating method was established through a stress study, wherein different methods of degradation (oxidation, hydrolysis, photolysis, and temperature) were studied simultaneously to determine the active ingredient hydrocortisone acetate, preservatives propyl parahydroxybenzoate, and methyl parahydroxybenzoate, antioxidant butylhydroxyanisole (BHA), and their degradation products in a semisolid dosage gel form. The proposed method was suitably validated using a Zorbax SB-Phenyl column and gradient elution. The mobile phase consisted of a mixture of methanol, acetonitrile, and water in different proportions according to a planned program at a flow rate of 1.5 mL/min. The diode array detector was set at 240 nm for the active substance and two preservatives,and 290 nm for BHA. The validation study was conducted according to International Conference on Harmonization guidelines for specificity, linearity, repeatability, precision, and accuracy. The method was usedfor QC of hydrocortisone acetate gel and for the stability studies with the aim of quantifying the active substance, preservatives, antioxidant, and degradation products. It has proved to be suitable as a fast and reliable method for QC.

scholarly journals Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Guaifenesin and Dextromethorphan Impurities in Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-12 ◽  
Author(s):  
Thummala V. Raghava Raju ◽  
Noru Anil Kumar ◽  
Seshadri Raja Kumar ◽  
Annarapu Malleswara Reddy ◽  
Nittala Someswara Rao ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
The Stability

A sensitive, stability-indicating gradient RP-HPLC method has been developed for the simultaneous estimation of impurities of Guaifenesin and Dextromethorphan in pharmaceutical formulations. Efficient chromatographic separation was achieved on a Sunfire C18, 250 × 4.6 mm, 5 µm column with mobile phase containing a gradient mixture of solvents A and B. The flow rate of the mobile phase was 0.8 mL min−1 with column temperature of 50°C and detection wavelength at 224 nm. Regression analysis showed an r value (correlation coefficient) greater than 0.999 for Guaifenesin, Dextromethorphan, and their impurities. Guaifenesin and Dextromethorphan formulation sample was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Guaifenesin was found stable and Dextromethorphan was found to degrade significantly in peroxide stress condition. The degradation products were well resolved from Guaifenesin, Dextromethorphan, and their impurities. The peak purity test results confirmed that the Guaifenesin and Dextromethorphan peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines with respect to specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness.

scholarly journals Stability-Indicating HPLC Method for isoflavones aglycones analysis from Trifolium pratense L. extract

2020 ◽  
Vol 4 (1) ◽  
pp. 28-38
Author(s):  
Simony Martiny ◽  
Mairique Waszczuk ◽  
Samuel Kaiser ◽  
Marina Cardoso Nemitz ◽  
Valquiria Linck Bassani
Keyword(s):  
Hplc Analysis ◽  
Trifolium Pratense ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Media ◽  
Biochanin A ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
The Stability

The purpose of this study was to develop and validate a fast HPLC stability-indicating method for simultaneously quantifying the four main isoflavones in Trifolium pratense. Validation procedures followed the ICH requirements for complex matrices. The stability-indicating tests were performed by exposing the isoflavones to conditions of forced degradation and further analysis for verifying the formation of degradation products and their possible interferences in the HPLC analysis. The major isoflavones of Trifolium pratense proved to be stable against acid and oxidative media, thermodegradation, and photodegradation. However, they proved to be unstable in alkaline media, even for short periods of exposure like 2h. In this condition, in addition to the peaks corresponding to isoflavones, the HPLC analysis showed the presence of three additional peaks which were eluted at different retention times to the reference substances, without interfering in the quantification of the four analytes of interest, formononetin, biochanin A, daidzein and genistein. The method was validated following ICH guidelines showing to be specific, linear, precise, accurate, and robust.This first report concerning a stability-indicating method revealed that the proposed HPLC method reliably quantify the isoflavones and separate them from the degradation products in a short time of analysis.

scholarly journals Stability-Indicating Validated HPLC Method for Analysis of Berberine Hydrochloride and Trimethoprim in Pharmaceutical Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Jing-Chun Wang ◽  
Qi Zhang ◽  
De-Fu Cai
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Berberine Hydrochloride ◽  
Stability Indicating ◽  
Relative Standard ◽  
The Stability

A stability-indicating HPLC method was developed and validated for the determination of berberine hydrochloride and trimethoprim in pharmaceutical dosage form in the presence of degradation products. The proposed RP-HPLC method utilizes an Agilent TC-C18, 4.6 mm × 250 mm, 5 μm, column using a mobile phase consisting of acetonitrile-50 mM potassium dihydrogen phosphate (30 : 70, v/v, pH adjusted to 3 with orthophosphoric acid) at a flow rate of 1.0 mL/min and UV detection at 271 nm. The linearity of berberine hydrochloride and trimethoprim was in the range of 2 to 60 μg/mL (r=0.9996) and 1 to 30 μg/mL (r=0.9995), respectively. Repeatability and intermediate precisions were also determined with percentage relative standard deviation (% RSD) less than 2.0%. The limits of detection were found to be 9.8 ng/mL for berberine hydrochloride and 2.5 ng/mL for trimethoprim. The mean recoveries for berberine hydrochloride and trimethoprim were 99.8 and 98.8%, respectively. The stability of the two drugs was determined under different conditions and the proposed method has shown effective separation for their degradation products. And the proposed assays method can thus be considered stability-indicating.

Stability of a pyrimethamine suspension compounded from bulk powder

2017 ◽  
Vol 74 (24) ◽  
pp. 2060-2064 ◽  
Author(s):  
Paul O. Lewis ◽  
David B. Cluck ◽  
Jessica D. Huffman ◽  
Amanda P. Ogle ◽  
Stacy D. Brown
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
Hplc Method ◽  
Stability Indicating ◽  
Color Changes ◽  
Stability Indicating Method ◽  
Bulk Powder ◽  
Subsequent Application ◽  
Temperature Ranges ◽  
The Stability

Abstract Purpose Development of a stability-indicating high-performance liquid chromatography (HPLC) method for pyrimethamine analysis, with subsequent application of that method to assess the 90-day stability of a pyrimethamine suspension compounded from bulk USP-grade pyrimethamine powder, is described. Methods A stability-indicating method of HPLC with ultraviolet detection specific to pyrimethamine was developed according to pharmacopeial recommendations and validated. The method was applied to investigate the stability of a 2-mg/mL pyrimethamine suspension in a vehicle consisting of Ora-Plus and Ora-Sweet (Perrigo) over a period of 90 days. Three replicate test preparations were stored at room temperature or refrigerated at 4.3–5.2 °C, and samples were analyzed in duplicate immediately after preparation and on study days 1, 2, 4, 7, 10, 14, 21, 30, 48, 60, 75, and 90. Results The 2-mg/mL suspension of pyrimethamine in Ora-Plus and Ora-Sweet retained 90–110% of the labeled potency to 90 days at both temperature ranges. However, color changes in the samples stored at room temperature observed at day 60 indicated that a beyond-use date less than 90 days from the preparation date should be specified when the suspension is to be stored at room temperature. Conclusion The study demonstrated that USP-grade pyrimethamine powder can be formulated as a 2-mg/mL suspension in a vehicle of Ora-Plus and Ora-Sweet and is stable when stored at room temperature and when refrigerated, in amber plastic bottles, for 48 and 90 days, respectively.

scholarly journals Stability-indicating derivative spectrophotometry method for the determination of biapenem in the presence of its degradation products

2011 ◽  
Vol 9 (1) ◽  
pp. 35-40 ◽  
Author(s):  
Judyta Cielecka-Piontek ◽  
Aran Lunzer ◽  
Anna Jelińska
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Subtraction Technique ◽  
Pharmaceutical Dosage Form ◽  
Zero Crossing ◽  
Stability Indicating ◽  
First Derivative ◽  
The Stability ◽  
Crossing Point

AbstractA first-derivative UV spectrophotometric method, with or without the subtraction technique, was developed for the determination of biapenem in pharmaceutical dosage form in the presence of its degradation products. The method was based on the measurement of first-derivative amplitudes at zero crossing point (λ = 312 nm) and the peak-to-zero technique and validated with regard to linearity, limits of detection and quantitation, selectivity and precision. The observed rate constants for the degradation of biapenem were comparable to those obtained in the stability-indicating HPLC method.

scholarly journals Development and validation of the stability-indicating LC-UV method for the determination of cefoselis sulphate

2012 ◽  
Vol 10 (1) ◽  
pp. 121-126 ◽  
Author(s):  
Przemysław Zalewski ◽  
Judyta Cielecka-Piontek ◽  
Anna Jelińska
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Kinetic Studies ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
The Stability ◽  
Development And Validation

AbstractThe stability-indicating LC assay method was developed and validated for quantitative determination of cefoselis sulphate in the presence of degradation products formed during the forced degradation studies. An isocratic, RP-HPLC method was developed with C-18 (250 × 4.6 mm, 5 µm) column and 12 mM ammonium acetate-acetonitrile (95:5 V/V) as a mobile phase. The flow rate of the mobile phase was 1.0 mL min−1. Detection wavelength was 260 nm and temperature was 30°C. Cefoselis similarly to other cephalosporins was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis and thermal degradation. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness. The method was applied successfully for identification and determination of cefoselis sulphate in pharmaceuticals and during kinetic studies.

Stability of Caffeine Injection in Intravenous Admixtures and Parenteral Nutrition Solutions

DICP ◽  
1989 ◽  
Vol 23 (6) ◽  
pp. 466-467 ◽  
Author(s):  
Milap C. Nahata ◽  
Josephine R. Zingarelli ◽  
Diane E. Durrell
Keyword(s):  
Amino Acids ◽  
Parenteral Nutrition ◽  
Potassium Chloride ◽  
Room Temperature ◽  
Hplc Method ◽  
Final Concentration ◽  
Stability Indicating ◽  
The Stability

Our objective was to determine the stability of caffeine base in intravenous admixtures and parenteral nutrition solutions at room temperature for 24 hours. Caffeine 10 mg/mL was used in this study. The admixtures included D5W; D5W with NaCl 0.2% injection; D5W with NaCl 0.2% and 20 mEq/L of potassium chloride injection; D10W injection; and D10W with NaCl 0.2% and 5 mEq/L of KCl injection. The parenteral nutrition solutions included 1.1% amino acids with electrolytes; 2.2% amino acids with electrolytes; and 4.25% amino acids with electrolytes. These parenteral nutrition solutions were prepared in D10W. Ten milliliters of caffeine were added to glass test tubes containing 10 mL of various solutions to yield a final concentration of 5 mg/mL. One milliliter aliquots were removed at 0, 2, 4, 8, and 24 hours and caffeine was measured by a stability-indicating HPLC method. The largest change in the concentrations of caffeine was 4.1 percent during the study period. Thus, caffeine injection is stable in various admixtures and parenteral nutrition solutions at room temperature for 24 hours.

scholarly journals Stability Study of Darunavir Ethanolate Tablets Applying a New Stability-Indicating HPLC Method

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Josilene Chaves Ruela Corrêa ◽  
Cristina Helena dos Reis Serra ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Raw Material ◽  
Forced Degradation ◽  
The Novel ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
The Stability ◽  
Darunavir Ethanolate

Chemical and physical degradation of drugs may result in altered therapeutic efficacy and even toxic effects. Therefore, the aim of this work was to study the stability of darunavir and to develop and validate a liquid chromatography (LC) method to determine darunavir in raw material and tablets in the presence of degradation products. The novel method showed to be linear from 6.0 to 21.0 μg/mL, with high precision (CV < 2%) and accuracy (recuperation of 99.64%). It is simple and reliable, free of placebo interferences. The robustness of the method was evaluated by a factorial design using seven different parameters. Forced degradation study was done under alkaline, acidic, and oxidative stress at ambient temperature and by heating. The LC method was able to quantify and separate darunavir and its degradation products. Darunavir showed to be unstable under alkaline, acid, and oxidative conditions. The novelty of this study is understanding the factors that affect darunavir ethanolate stability in tablets, which is the first step to unravel the path to know the degradation products. The novel stability-indicating method can be used to monitor the drug and the main degradation products in low concentrations in which there is linearity.

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