Beyond-Use Dates Assignment for Pharmaceutical Preparations: Example of Low-Dose Amiodarone Capsules

2021 ◽  
pp. 875512252110155
Author(s):  
Damien Brun ◽  
Christophe Curti ◽  
Edouard Lamy ◽  
Christophe Jean ◽  
Pierre Bertault-Peres ◽  
...  
Keyword(s):  
Microcrystalline Cellulose ◽  
Low Dose ◽  
Pharmaceutical Preparations ◽  
The United States ◽  
Stability Study ◽  
Potential Drug ◽  
Stability Studies ◽  
United States Pharmacopoeia ◽  
Amiodarone Hydrochloride

Background: Beyond-use dates (BUDs) in compounding practice are assigned from stability studies. The United States Pharmacopoeia (USP 42 NF 37) suggested to assign a 6 months BUD for dry oral forms. A new pediatric formula of amiodarone capsules was implemented in our hospital, with 3 dosages (5 mg, 20 mg, and 50 mg). Objective: BUD of these new formulas had to be determined by stability study. Methods: The method for the determination of amiodarone content was validated to be stability indicating, and a stability study was performed. Different excipients commonly used for capsule compounding were compared. Results: We found that, with microcrystalline cellulose as excipient, 50 mg amiodarone capsules were stable for 1 year, whereas 5 mg and 20 mg capsules were not. This difference was studied, and lactose or mannitol were found to be better excipients for 5 mg amiodarone capsules, despite their potential side effects. A potential drug-excipient interaction between microcrystalline cellulose and amiodarone hydrochloride is described. Conclusion: Amiodarone hydrochloride/microcrystalline cellulose capsules have a BUD of 1 month for 5 mg capsules, 6 months for 20 mg, and 1 year for 50 mg.

scholarly journals Potentiometric determination of captopril in pharmaceutical formulations

2003 ◽  
Vol 28 (1) ◽  
pp. 39-44 ◽  
Author(s):  
P. R. da S. Ribeiro ◽  
A. O. Santini ◽  
H. R. Pezza ◽  
L. Pezza
Keyword(s):  
Low Cost ◽  
Standard Procedure ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Magnesium Stearate ◽  
The United States ◽  
United States Pharmacopoeia ◽  
Glass Ph Electrode ◽  
Tablet Dosage

A simple, precise, rapid and low-cost potentiometric method for captopril determination in pure form and in pharmaceutical preparations is proposed. Captopril present in tablets containing known quantity of drug was potentiometrically titrated in aqueous solution with NaOH using a glass pH electrode, coupled to an autotitrator. No interferences were observed in the presence of common components of the tablets as lactose, microcrystalline cellulose, croscarmellose sodium, starch and magnesium stearate. The analytical results obtained by applying the proposed method compared very favorably with those obtained by the United States Pharmacopoeia Standard procedure. Recovery of captopril from various tablet dosage formulations range from 98.0 to 102.0%.

scholarly journals Validation of an HPLC Assay Method for Routine QC Testing and Stability Study of Compounded Low-Dose Capsules of Acetylsalicylic Acid

2018 ◽  
Vol 3 (4) ◽  
pp. 199-206
Author(s):  
Nelly Lonca ◽  
Fabienne Maillard ◽  
Géraldine Leguelinel ◽  
Tahmer Sharkawi ◽  
Ian Soulairol
Keyword(s):  
Acetylsalicylic Acid ◽  
Orthophosphoric Acid ◽  
Low Dose ◽  
Stability Study ◽  
Assay Method ◽  
Stability Studies ◽  
Physicochemical Stability ◽  
Hospital Pharmacies ◽  
Provocation Testing ◽  
Low Dosage

Abstract Background The intolerance to Acetylsalicylic Acid (ASA) can be detected by conducting oral provocation testing (OPT), which is to gradually introduce low doses of ASA. To perform this test, hospital pharmacies compound small batches of different low-dosage ASA capsules. This work aims to validate a method for fast HPLC-UV assay that allows routine quality control and physicochemical stability studies of capsules. Methods The chromatographic separation is performed using a C18 column Kinetex (100 A, 50×4.6 mm, 2.6 µm) equipped with a precolumn C18. Separation is achieved using a mobile phase composed of water-acetonitrile-orthophosphoric acid (68:32:0.2 v/v/v) at a flow rate of 0.8 mL/min and UV detection at 237 nm. Results Validation shows that the method was suitable for routine analysis and could be used to perform stability studies. Conclusions The 5, 25, 100 and 250 mg dosed capsules show acceptable stability over 12 months, while the 1 mg dosed capsule show an unacceptable degradation of more than 15 % after 3 months. Therefore, hospital pharmacy can plan the manufacture of capsules and anticipate the requests of doctors.

scholarly journals Spectrofluorometric Determination of Verapamil Hydrochloride in Pharmaceutical Preparations and Human Plasma Using Organized Media: Application to Stability Studies

2006 ◽  
Vol 89 (6) ◽  
pp. 1565-1572 ◽  
Author(s):  
Mohamed Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Amina Abdelsalam
Keyword(s):  
Human Plasma ◽  
Biological Fluids ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Stability Studies ◽  
Verapamil Hydrochloride ◽  
Spiked Human Plasma

Abstract A highly sensitive spectrofluorometric method was developed for the determination of verapamil hydrochloride (VP HCl) in pharmaceutical formulations and biological fluids. The proposed method is based on investigation of the fluorescence spectral behavior of VP HCl in micellar systems, such as sodium dodecyl sulfate (SDS) and β-cyclodextrin (β-CD). In aqueous solutions of borate buffer of pH 9 and 8.5, VP HCl was well incorporated into SDS and β-CD, respectively, with enhancement of its native fluorescence. The fluorescence was measured at 318 nm after excitation at 231 nm. The fluorescence intensity enhancements were 183 and 107% in SDS and in β-CD, respectively. The fluorescence-concentration plots were rectilinear over the range of 0.020.2 and 0.020.25 μg/mL, with lower detection limits of 5.58 × 103 and 3.62 × 103 μg/mL in SDS and β-CD, respectively. The method was successfully applied to the analysis of commercial tablets and the results were in good agreement with those obtained with the official method. The method was further applied to the determination of VP HCl in real and spiked human plasma. The mean % recoveries in the case of spiked human plasma (n 4) was 92.59 3.11 and 88.35 2.55 using SDS and β-CD, respectively, while that in real human plasma (n 3) was 90.17 6.93 and 89.17 6.50 using SDS and β-CD, respectively. The application of the method was extended to the stability studies of VP HCl after exposureto ultraviolet radiation and upon oxidation with hydrogen peroxide.

scholarly journals A Sensitive Spectrophotometric Determination of Ritodrine, Pentazocine, Isoxsuprine Hydrochlorides and Amoxicillin in Pure and Pharmaceutical Samples

2008 ◽  
Vol 5 (1) ◽  
pp. 100-106 ◽  
Author(s):  
H. D. Revanasiddappa ◽  
M. A. Veena
Keyword(s):  
Acid Medium ◽  
The United States ◽  
Molar Absorptivity ◽  
United States Pharmacopoeia ◽  
Hydrochloric Acid Medium ◽  
Subsequent Determination ◽  
Highly Sensitive ◽  
Coloured Complex ◽  
Chloramine T

A simple, accurate and highly sensitive spectrophotometric method for the determination of ritodrine hydrochloride (RTH), pentazocine hydrochloride (PZH), isoxsuprine hydrochloride (ISH) and amoxicillin (AMX) is described. The method is based on the oxidation of the studied drugs by a known excess of chloramine – T (CAT) in hydrochloric acid medium and subsequent determination of the unreacted oxidant by reacting it with iodide in the same acid medium liberates iodine, which subsequently react with starch to form a stable starch-iodine complex. The reacted oxidant corresponds to the drug content. The coloured complex exhibits a maximum absorption at 590 nm. The apparent molar absorptivity values and Sandell’s sensitivity values are in the range 6.96x104- 1.43x105L mol–1cm–1and 2.45-4.30 ng cm–2, respectively. The method was successfully applied to the studied drugs in their dosage forms. The results are reproducible within ±1% and compare favorably with those of official methods of British Pharmacopoeia and the United States Pharmacopoeia.

scholarly journals Enantiomeric Determination of Omeprazole and Esomeprazole by a Developed and Validated Chiral HPLC Method and Stability Studies by Microthermal Analysis

2018 ◽  
Vol 16 (2) ◽  
pp. 221-233
Author(s):  
Asma Rahman ◽  
Mohammad Rashedul Haque ◽  
Md Zakir Sultan ◽  
M Muhibur Rahman ◽  
Mohammad A Rashid
Keyword(s):  
High Sensitivity ◽  
The United States ◽  
Hplc Method ◽  
Stability Study ◽  
Chiral Hplc ◽  
Scanning Calorimetry ◽  
Average Percentage ◽  
Relative Standard ◽  
Physical And Chemical

A rapid, accurate, precise, stability indicating and enantioselective chiral HPLC method was developed and validated for the quantitative (S)- and (R)- omeprazole in omeprazole formulations along with determination of enantiomeric purity of (S)- omeprazole in esomeprazole formulations according to the guidelines of the United States of Pharmacopeia (USP) and International Conference on Harmonization (ICH). The chromatographic separation was achieved with n-hexane/ 2-propanol/ acetic acid/ triethylamine (100 : 20 : 0.2 : 0.1, v/v) at a flow rate of 1.2 ml/min on Chiralcel OD-H and detected at 300 nm. The method showed good linearity, high sensitivity with detection limit (LOD) of 0.71 and 1.16 μg/ml and quantitation limit (LOQ) of 2.16 and 3.51 μg/ml for (S)- and (R)- omeprazole, respectively. The average percentage of recovery was found to be 100.85% to 101.36% for (S)- and 99.81% to 101.62% for (R)- omeprazole. The average percentage of relative standard deviation (% RSD) for intra- and inter- day precision were found to be 0.05% and 0.19% for (S)- and 0.03% and 0.13% for (R)- omeprazole, respectively. Stability study was performed under stress conditions. Microthermal analysis of omeprazole was also performed by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM) to assess the physical and chemical behavior of the drug. The method was successfully applied to the quantitation of (S)- and (R)- omeprazole for omeprazole and as well as determination of (S)- omeprazole purity for esomeprazole formulations.Dhaka Univ. J. Pharm. Sci. 16(2): 221-233, 2017 (December)

scholarly journals POTENTIAL OF CELLULASE OF PENICILLIUM VERMICULATUM FOR PREPARATION AND CHARACTERIZATION OF MICROCRYSTALLINE CELLULOSE PRODUCED FROM α-CELLULOSE OF KAPOK PERICARPIUM (CEIBA PENTANDRA)

2019 ◽  
pp. 92-97
Author(s):  
HERMAN SURYADI ◽  
SUTRIYO ◽  
Mira Junnisa ◽  
YULIANITA PRATIWI INDAH LESTARI
Keyword(s):  
United States ◽  
Microcrystalline Cellulose ◽  
Cellulase Activity ◽  
The United States ◽  
X Ray Diffraction ◽  
Clear Zone ◽  
United States Pharmacopoeia ◽  
X Ray ◽  
Particle Size Analyzer

Objective: This study aimed to find psychochemical properties of microcrystalline cellulose (MCC) obtained from α-cellulose kapok pericarpium. Methods: The cellulase activity was screened by clear zone and sugar reduction method. The enzym from selected mold was purified by diethylaminoethyl (DEAE) chromatography. α-cellulose of kapok pericarpium was hydrolyzed using the purified cellulase enzymes. Microcrystalline cellulose (MCC) identified by Fourier transform infrared (FTIR) spectrometry, and qualitative analysis test. The samples were characterized for pH test, x-ray diffraction (XRD), and particle size analyzer (PSA). Results: The optimum cellulase activity was shown by Penicillium vermiculatum. It’s clear zone diameter around 3 cm and the cellulase activity was 67.73±0.25 mU/ml. The strongest cellulase activity was detected from 1st fraction (P1) out of 6 column fractions with optimum activity at 1.177±2 mU/ml. The optimal conditions for microcrystalline cellulose (MCC) preparation were at 50 ˚C, for 2 ours, using 20 ml of acetate buffer pH 5 and 2 ml of cellulase enzyme. Microcrystalline cellulose (MCC) obtained at 78% w/w and its FTIR spectrum and x-ray diffractogram similar to reference while the pH of MCC was fulfilled requirements of The United States Pharmacopoeia 2007. Conclusion: The use of purified enzyme of cellulase has succeded in microcrystalline cellulose (MCC) preparation andmicrocrystalline cellulose (MCC) obtained was 78% w/w, with similar characteristics to reference (Avicel PH 101) and the pH of MCC was fulfilled requirements of The United States Pharmacopoeia 2007.

A fast spectrofluorimetric method for determination of carbinoxamine maleate in the nano-molar range. Application to pharmaceutical preparations, biological fluids and stability studies

2018 ◽  
Vol 10 (31) ◽  
pp. 3851-3858 ◽  
Author(s):  
Fatma Ahmed Aly ◽  
Nahed EL-Enany ◽  
Heba Elmansi ◽  
Amany Nabil
Keyword(s):  
Human Plasma ◽  
Biological Fluids ◽  
Pharmaceutical Preparations ◽  
Pure Form ◽  
Stability Studies ◽  
Spiked Human Plasma ◽  
Spectrofluorimetric Method

Carbinoxamine maleate (CBX), which is a common ingredient of cold and cough treatment preparations, is determined by a sensitive, simple and convenient spectrofluorimetric method in its pure form, pharmaceutical preparations and spiked human plasma.

scholarly journals Spectrophotometric determination of diclofenac in pharmaceutical preparations assisted by microwave oven

2005 ◽  
Vol 30 (1) ◽  
pp. 29-36 ◽  
Author(s):  
E. G. Ciapina ◽  
A. O. Santini ◽  
P. L. Weinert ◽  
M. A. Gotardo ◽  
H. R. Pezza ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Low Cost ◽  
Standard Procedure ◽  
Pharmaceutical Preparations ◽  
Magnesium Stearate ◽  
The United States ◽  
Molar Absorptivity ◽  
Heating Time ◽  
Limit Of Quantification

In this work, an effective and low-cost method for the determination of sodium or potassium diclofenac is proposed in its pure form and in their pharmaceutical preparations. The method is based on the reaction between diclofenac and tetrachloro-p-benzoquinone (p-chloranil), in methanol medium. This reaction was accelerated by irradiating of reactional mixture with microwave energy (1100 W) during 27 seconds, producing a charge transfer complex with a maximum absorption at 535 nm. The optimal reaction conditions values such as reagent concentration, heating time and stability of the reaction product were determined. Beer's law is obeyed in a concentration range from of 1.25x10-4 to 2.00x10-3 mol l-1 with a correlation coefficient of 0.9993 and molar absorptivity of 0.49 x10³ l mol-1 cm-1. The limit of detection (LOD) was 1.35x10-5 mol l-1 and the limit of quantification (LOQ) was 4.49x10-5 mol l-1. In the presence of the common excipients, such as glucose, lactose, talc, starch, magnesium stearate, sodium sulphite, titanium dioxide, polyethyleneglycol, polyvinylpirrolidone, mannitol and benzilic alcohol no interferences were observed. The analytical results obtained by applying the proposed method compare very favorably with those given by the United States Pharmacopeia standard procedure. Recoveries of diclofenac from various pharmaceutical preparations were within 95.9% to 103.3%, with standard deviations ranging from 0.2% to 1.8%.

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