Validation of the framycetin sulfate determination technique by HPLC in a Framidex medicinal preparation

2020 ◽  
Vol 86 (6) ◽  
pp. 73-78
Author(s):  
D. D. Gapparov ◽  
Z. A. Smanova ◽  
Y. V. Timchenko ◽  
A. V. Pirogov
Keyword(s):  
Medicinal Preparation ◽  
Good Manufacturing Practice ◽  
Variation Coefficient ◽  
Intermediate Precision ◽  
Average Value ◽  
Limit Of Determination ◽  
Validation Criteria ◽  
Derivatizing Agent ◽  
Order Of Magnitude

A method for determination of framycetin sulfate in a Framidex preparation (eye and ear drops) by HPLC-UV (λ = 365 nm) using 2, 4-dinitrofluorobenzene as a derivatizing agent has been developed The characteristics of analytical methods determined for the purpose of their validation and relevant criteria for the validity of validated methods with the goal of the quality control of drugs (pharmaceutical substances and drugs) are presented. According to the results of an intralaboratory experiment on the validation assessment of the method by the parameters of the specificity, limit of determination (LOD), linearity, precision and laboratory accuracy, it is shown that the LOD decreases by an order of magnitude, the correlation coefficient is not less than 0.99 correctness (average value — 97.5 – 102.5%; variation coefficient — not more than 2.0%; the confidence range should include 100% of values), convergence (variation coefficient — not more than 1.5%), intermediate precision (variation coefficient — not more than 1.5%). It is shown that the obtained values of metrological characteristics do not exceed the validation criteria and the developed method matches all the well-known requirements of GMP (Good Manufacturing Practice).

scholarly journals Intra-Laboratory Validation of Alpha-Galactosidase Activity Measurement in Dietary Supplements

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1566
Author(s):  
Elena Fabris ◽  
Michela Bulfoni ◽  
Alessandro Nencioni ◽  
Emanuele Nencioni
Keyword(s):  
Dietary Supplements ◽  
Good Manufacturing Practice ◽  
Activity Measurement ◽  
Intermediate Precision ◽  
Method Performance ◽  
Intestinal Gas ◽  
Technical Requirements ◽  
Ich Guidelines ◽  
Alpha Galactosidase

Introduction: Alpha-galactosidase (α-Gal) is an enzyme responsible for the hydrolyzation of glycolipids and glycoprotein commonly found in dietary sources. More than 20% of the general population suffers from abdominal pain or discomfort caused by intestinal gas and by indigested or partially digested food residuals. Therefore, α-Gal is used in dietary supplements to reduce intestinal gases and help complex food digestion. Marketed enzyme-containing dietary supplements must be produced in accordance with the Food and Drug Administration (FDA) regulations for Current Good Manufacturing Practice (cGMPs). Aim: in this work we illustrated the process used to develop and validate a spectrophotometric enzymatic assay for α-Gal activity quantification in dietary supplements. Methods: The validation workflow included an initial statistical-phase optimization of materials, reagents, and conditions, and subsequently a comparative study with another fluorimetric assay. A final validation of method performance in terms of specificity, linearity, accuracy, intermediate-precision repeatability, and system precision was then executed. Results and conclusions: The proven method achieved good performance in the quantitative determination of α-Gal activity in commercial food supplements in accordance with the International Council for Harmonisation of Technical Requirements for Pharmaceuticals (ICH) guidelines and is suitable as a rapid in-house quality control test.

scholarly journals Sensitivity of the Groundwater Mound Model for Predicting Mire Topography

1987 ◽  
Vol 18 (4-5) ◽  
pp. 193-202 ◽  
Author(s):  
Pauline E. Kneale
Keyword(s):  
Hydraulic Conductivity ◽  
Limited Data ◽  
Average Value ◽  
Error Band ◽  
Order Of Magnitude ◽  
Equilibrium Profile ◽  
Using Data ◽  
Sensitive Parameters ◽  
Objective Determination

The Dupuit-Forcheimer model for groundwater mounds has been proposed to explain the morphology of raised peat mires. This paper discusses the sensitivity of the model as a predictor for mire profiles using data from a raised Irish mire where an attempt was made to reconstruct the equilibrium profile. The most sensitive parameters are shown to be hydraulic counductivity and net recharge. Detailed measurements of saturated hydraulic conductivity show significant spatial variability, which is correlated with mire stratigraphy. Objective determination of an average value for modelling would have an error band of an order of magnitude which is unsatisfactory for prediction. Net recharge is calculated from the water balance but parameters like overlandflow must be estimated, usually from limited data, making the proposed value suspect. This model may be helpful for mire description but its variables cannot be specified accurately enough for predictive purposes.

Development of a method for multielemental determination in water by EDXRF with radioisotopic source of 238Pu.

2019 ◽  
Vol 7 (2A) ◽  
Author(s):  
Camilo Fuentes Serrano ◽  
Juan Reinaldo Estevez Alvares ◽  
Alfredo Montero Alvarez ◽  
Ivan Pupo Gonzales ◽  
Zahily Herrero Fernandez ◽  
...  
Keyword(s):  
Thin Layer ◽  
Expanded Uncertainty ◽  
Considerable Decrease ◽  
X Ray ◽  
Precipitation Efficiency ◽  
Method Of Determination ◽  
Sensitivity Curves ◽  
Order Of Magnitude ◽  
Metrological Parameters

A method for determination of Cr, Fe, Co, Ni, Cu, Zn, Hg and Pb in waters by Energy Dispersive X Ray Fluorescence (EDXRF) was implemented, using a radioisotopic source of 238Pu. For previous concentration was employed a procedure including a coprecipitation step with ammonium pyrrolidinedithiocarbamate (APDC) as quelant agent, the separation of the phases by filtration, the measurement of filter by EDXRF and quantification by a thin layer absolute method. Sensitivity curves for K and L lines were obtained respectively. The sensitivity for most elements was greater by an order of magnitude in the case of measurement with a source of 238Pu instead of 109Cd, which means a considerable decrease in measurement times. The influence of the concentration in the precipitation efficiency was evaluated for each element. In all cases the recoveries are close to 100%, for this reason it can be affirmed that the method of determination of the studied elements is quantitative. Metrological parameters of the method such as trueness, precision, detection limit and uncertainty were calculated. A procedure to calculate the uncertainty of the method was elaborated; the most significant source of uncertainty for the thin layer EDXRF method is associated with the determination of instrumental sensitivities. The error associated with the determination, expressed as expanded uncertainty (in %), varied from 15.4% for low element concentrations (2.5-5 μg/L) to 5.4% for the higher concentration range (20-25 μg/L).

The Development of a Turbidimetric Method for the Quantitative Determination of Antibiotics of the Aminoglycoside Group in Medications

2020 ◽  
Vol 65 (7-8) ◽  
pp. 37-41
Author(s):  
E. N. Semenova ◽  
S. I. Kuleshova ◽  
E. I. Sakanyan
Keyword(s):  
Quantitative Determination ◽  
Quality Assessment ◽  
Aminoglycoside Antibiotics ◽  
Metrological Characteristics ◽  
Streptomycin Sulfate ◽  
Turbidimetric Method ◽  
Validation Criteria ◽  
Validation Parameters ◽  
Validation Tests

A method for the quantitative determination of streptomycin sulfate in medicines by the turbidimetric method has been developedand validated. Based on the results of the experiments, it was found that the metrological characteristics of such validation parameters of the method as linearity, precision, and correctness do not exceed the validation criteria. Linearity was noted in the range of streptomycin concentrations from 3.75 to 8.43 μg/ml. The results of validation tests of the method for the quantitative determination of streptomycin indicate the prospects and feasibility of introducing the turbidimetric method into the domestic system for standardization and quality assessment of aminoglycoside antibiotics.

Titration of sulphates and lead using lead ion selective electrode

1981 ◽  
Vol 46 (2) ◽  
pp. 368-376 ◽  
Author(s):  
Josef Veselý
Keyword(s):  
Ionic Strength ◽  
Electrode Surface ◽  
Salt Content ◽  
Ion Selective Electrode ◽  
Lead Ion ◽  
Selective Electrode ◽  
Limit Of Determination ◽  
Total Salt Content ◽  
Automatic Titration

Titration of sulphates with lead perchlorate employing lead ion selective electrode indication was studied using additions of various organic solvents at different pH' and ionic strength values. As the optimum emerged systems with 60-70% 1,4-dioxane, pH' 5.3-5.6. After dehydration with sodium hydroxide, dioxane must be freed from the electrode surface-oxidizing impurities by their reduction with sodium metal and subsequent distillation. The method was applied to determination of sulphates in mountain spring waters. Units of ppm can be determined; the limit of determination, however, depends considerably on the content of dioxane, total salt content in the sample, and speed of the semi-automatic titration. Lead can be determined with EDTA in concentrations down to c(Pb2+) = 5 . 10-6 mol l-1.

Spectrophotometric Determination of Raceophenidol in Feed at Very Low Levels

1968 ◽  
Vol 51 (4) ◽  
pp. 752-755
Author(s):  
Edward L Pratt ◽  
Morris E Auerbach
Keyword(s):  
Spectrophotometric Determination ◽  
Growth Promotion ◽  
Ultraviolet Spectrum ◽  
Average Value ◽  
Collaborative Studies ◽  
Low Levels ◽  
Concentration Levels

Abstract Raceophenidol in feed at concentration levels intended for growth promotion of poultry can be estimated by a curvature inversion measurement related to the ultraviolet spectrum of derived p-methylsulfonylbenzaldehyde. The drug can be accurately measured at the 0.0005% level. Collaborative studies on the method showed an average value of 94 ± 10% of claim. The method is recommended for adoption as official, first action.

scholarly journals Determination of vertical dimension of occlusion by using the phonetic vowel "O" and "E"

2015 ◽  
Vol 72 (2) ◽  
pp. 123-131 ◽  
Author(s):  
Marko Igic ◽  
Nebojsa Krunic ◽  
Ljiljana Aleksov ◽  
Milena Kostic ◽  
Aleksandra Igic ◽  
...  
Keyword(s):  
Cognitive Functions ◽  
Complete Denture ◽  
Reference Points ◽  
Vertical Dimension ◽  
Entire Sample ◽  
Average Value ◽  
Significant Difference ◽  
The Relationship

Background/Aim. The vertical dimension of occlusion is a very important parameter for proper reconstruction of the relationship between the jaws. The literature describes many methods for its finding, from the simple, easily applicable clinically, to quite complicated, with the use of one or more devices for determination. The aim of this study was to examine the possibility of determining the vertical dimension of occlusion using the vocals ?O? and ?E? with the control of values o btained by applying cognitive functions. Methods. This investigation was performed with the two groups of patients. The first group consisted of 50 females and 50 males, aged 18 to 30 years. In this group the distance between the reference points (on top of the nose and chin) was measured in the position of the mandible in the vertical dimension of occlusion, the vertical dimension at rest and the pronunciation of the words ?OLO? and ?ELE?. Checking the correctness of the particular value for the word ?OLO? was also performed by the phonetic method with the application of cognitive exercises when the patients counted from 89 to 80. The obtained difference in the average values i n determining the vertical dimension of occlusion and the ?OLO? and ?ELE? in the first group was used as the reference for determining the vertical dimension of occlusion in the second group of patients. The second group comprised of 31 edentulous persons (14 females and 17 males), aged from 54 to 85 years who had been made a complete denture. Results. The average value obtained for the vertical dimension of rest for the entire sample was 2.16 mm, for the word ?OLO? for the entire sample was 5.51 mm and for the word ?ELE? for the entire sample was 7.47 mm. There was no statistically significant difference between the genders for the value of the vertical dimension at rest, ?ELE? and ?OLO?. There was a statistically significant difference between the values f or the vertical dimension at rest, ?OLO? and ?ELE? for both genders. There was a statistically significant correlation between the value for the vertical dimension at rest, ?OLO? and ?ELE?, for both groups of subjects. Conclusion. Determining the vertical dimension of occlusion requires 5.5 mm subtraction from the position of the mandible in pronunciation of the word ?OLO? or 7.5 mm in pronunciation of the word ?ELE?.

scholarly journals Fluorescent Orthopalladated Complexes of 4-Aryliden-5(4H)-Oxazolones from the Kaede Protein: Synthesis and Characterization

Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1238
Author(s):  
Eduardo Laga ◽  
David Dalmau ◽  
Sofía Arregui ◽  
Olga Crespo ◽  
Ana I. Jimenez ◽  
...  
Keyword(s):  
Intramolecular Interactions ◽  
Ortho Position ◽  
Fluorescent Properties ◽  
Ancillary Ligands ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Fluorescence Measurements ◽  
Anionic Ligands ◽  
Order Of Magnitude

The goal of the work reported here was to amplify the fluorescent properties of 4-aryliden-5(4H)-oxazolones by suppression of the hula-twist non-radiative deactivation pathway. This aim was achieved by simultaneous bonding of a Pd center to the N atom of the heterocycle and the ortho carbon of the arylidene ring. Two different 4-((Z)-arylidene)-2-((E)-styryl)-5(4H)-oxazolones, the structures of which are closely related to the chromophore of the Kaede protein and substituted at the 2- and 4-positions of the arylidene ring (1a OMe; 1b F), were used as starting materials. Oxazolones 1a and 1b were reacted with Pd(OAc)2 to give the corresponding dinuclear orthometalated palladium derivates 2a and 2b by regioselective C–H activation of the ortho-position of the arylidene ring. Reaction of 2a (2b) with LiCl promoted the metathesis of the bridging carboxylate by chloride ligands to afford dinuclear 3a (3b). Mononuclear complexes containing the orthopalladated oxazolone and a variety of ancillary ligands (acetylacetonate (4a, 4b), hydroxyquinolinate (5a), aminoquinoline (6a), bipyridine (7a), phenanthroline (8a)) were prepared from 3a or 3b through metathesis of anionic ligands or substitution of neutral weakly bonded ligands. All species were fully characterized and the X-ray determination of the molecular structure of 7a was carried out. This structure has strongly distorted ligands due to intramolecular interactions. Fluorescence measurements showed an increase in the quantum yield (QY) by up to one order of magnitude on comparing the free oxazolone (QY < 1%) with the palladated oxazolone (QY = 12% for 6a). This fact shows that the coordination of the oxazolone to the palladium efficiently suppresses the hula-twist deactivation pathway.

scholarly journals Concurrent chromatographic determination of pseudoephedrine and loratadine from combination syrups and tablets

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Imad Osman Abu Reid
Keyword(s):  
Ammonium Acetate ◽  
Chemical Properties ◽  
Chromatographic Determination ◽  
Analytical Challenge ◽  
Intermediate Precision ◽  
Box Behnken Design ◽  
Complex Samples ◽  
System Suitability ◽  
Nonpolar Compounds

Abstract Background Chromatographic separation of polar and nonpolar compounds when presented in combined dosage forms has always been considered as great analytical challenge. Separation and retention of both polar and nonpolar compounds by the same stationary phase can be a useful approach for analyses of complex samples with such a difference in chemical properties. Loratadine (nonpolar) and pseudoephedrine (polar) are typical examples of this situation. Results The Box–Behnken design was used to optimize the separation process, an efficient separation of loratadine and pseudoephedrine was achieved within 6 min; employing a mixture of 16.0 mM ammonium acetate buffer (pH 4.5) and acetonitrile (23:77, v/v) as isocratic mobile phase, pumped at 1.0 mL/min through a Zorbax cyanopropyl column (250 mm × 4.6 mm, 5 μm), the analytes were detected at 250 nm. Under the same conditions, separation of sodium benzoate preservative co-formulated with the two analytes in syrup formulation was also achieved. The calibration curve demonstrated excellent linearity in the range of 24.6–123.2 μg/mL and 594.8–2974.0 μg/mL for loratadine and pseudoephedrine, respectively with determination coefficient (r2) > 0.999. Conclusion The method’s accuracy bias < 2.0%, repeatability and intermediate precision (%RSD < 2.0%) were verified. In addition, system suitability parameters were found within the acceptable limits. Satisfactory results were obtained upon the application of the validated method to the analysis of commercial tablet and syrup formulations.

Expected Improvement in the Determination of G Using an X Pendulum

1997 ◽  
Vol 12 (11) ◽  
pp. 1967-1974 ◽  
Author(s):  
Kazuaki Kuroda ◽  
Mark A. Barton ◽  
Atsushi Onae ◽  
Yukinobu Miki
Keyword(s):  
Gravitational Constant ◽  
New Technique ◽  
Expected Improvement ◽  
Order Of Magnitude ◽  
Experimental Errors ◽  
A New Technique ◽  
Newtonian Gravitational Constant

We propose the application of a new technique, the X pendulum, to determine the Newtonian gravitational constant G. We evaluate the likely experimental errors for configurations realizable with existing technologies and show that improvement of the accuracy by an order of magnitude or more is possible.

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