Wyniki wyszukiwania - Biblioteka Nauki

1

Development and validation of a stability-indicating HPTLC method for analysis of 3-acetyl-11-keto-β-boswellic acid in a herbal extract and a nanoparticles formulation

100%

Goel A. , Goel R. , Jain G. K. , Singh R. M. , Ahmad F. J. , Singh G. N.

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2008

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tom Vol. 20, no. 3

497-511

EN

A new, specific, sensitive, selective, precise, and reproducible high-performance thin-layer chromatographic (HPTLC) method has been established for study of the stability of 3-acetyl-11-keto-β-boswellic acid (AKBA). HPTLC was performed on aluminium foil plates coated with 200 µm silica gel 60F 254 . Linear ascending development with toluene-ethyl acetate 7:3 ( v/v ) was performed at room temperature (25 š 2°C) in a twin-trough glass chamber saturated with mobile phase vapour. Compact bands ( R 0.52 š 0.02) were obtained for AKBA. Spectrodensitometric scanning was performed in absorbance mode at 250 nm. Linear regression analysis of the calibration plots showed there was a good linear relationship ( r 2 = 0.9989 š 0.0002) between peak area and concentration in the range 200-1200 ng band -1 . The method was validated for precision, recovery, robustness, specificity, and detection and quantification limits, in accordance with ICH guidelines. The limits of detection and quantification were 3.06 and 9.29 ng band -1, respectively. The recovery of the method was 99.35-100.21%. AKBA was subjected to various stress test conditions - acid and alkali hydrolysis, oxidation, photodegradation, and dry and wet heat treatment. Degradation products were well resolved from the pure drug with significantly different R F values. Statistical analysis showed the method could be successfully applied for the estimation of AKBA in herbal extract and in nanoparticles. Because the method could effectively separate the drug from its degradation products, it can be regarded as stability-indicating.

2

Procedura oznaczania pierwiastków we włosach

100%

Chodorowska A. , Lisowski W. , Stela M.

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2000

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tom R. 5, nr 2

30-31

3

Validated RP-HPLC analysis of irinotecan HCl in the bulk material and in pharmaceutical formulations

100%

Shende P. , Gaud R.

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2009

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tom Vol. 21, no. 1

71-82

EN

An isocratic reversed-phase high-performance liquid chromatographic (RPHPLC) method for analysis of irinotecan HCl has been developed and validated. Separation was achieved on a C 18 column with potassium dihydrogen phosphate buffer (pH adjusted to 3.5 with orthophosphoric acid)-acetonitrile-methanol 55:25:20 ( v/v ) as mobile phase at a flow rate of 1.0 mL min -1. UV detection was performed at 254 nm. The method is simple, sensitive, rapid, and selective, and linear over the range 30-70 µg mL -1 for assay of irinotecan HCl. The precision of the assay method was below 1.0% RSD. Mean recovery was in the range 98.0-102.0%. Recovery of the active pharmaceutical ingredient from dosage forms ranged from 99.0 to 101.0. The method is useful for quality control in bulk manufacture and of the pharmaceutical formulation.

4

RP-HPLC method for analysis of related substances in amoxicillin drug substance

100%

Raju C. B. V. N. , Sharma H. K. , Rao C. S. , Rao G. N.

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2009

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tom Vol. 21, no. 1

57-70

EN

Linear gradient HPLC on a C 8 column has been used for separation of individual related substances of amoxicillin listed in the European Pharmacopoeia and a newly identified degradation impurity. The USP plate count for the amoxicillin peak was more than 3000 and USP tailing for the same peak was less than 2.0. Forced degradation studies were conducted on amoxicillin drug substance using ICH stress study guidelines to demonstrate the specificity and stability-indicating nature of the method. A new impurity observed after thermal and alkaline degradation was identified as N -pivaloylamoxicillin. The LOD and LOQ for individual related substances were below 0.045 and 0.086% ( w/w ), respectively. The method was fully validated in accordance with ICH analytical method validation guidelines. The results of the study prove the method is specific, precise, linear, robust, and can be used for evaluation of the stability of amoxicillin drug substance.

5

PURITY DETERMINATION OF THE STARTING MATERIALS USED IN THE SYNTHESIS OF PHARMACEUTICAL SUBSTANCES

88%

Groman A. , Stolarczyk E. , Mucha M.

Acta Poloniae Pharmaceutica - Drug Research

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2019

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tom 76

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nr 1

29-35

EN

High requirements on the API quality mean that the quality control of the starting material is crucial to the manufacturing process of drug substances. Three sensitive methods for the purity determination of the following starting materials: ethylene glycol (method I), 3-acetylpyridine (method II) and 4-chloromethyl-5-methyl-1,3-dioxol-2-one (method III) used in the synthesis of selected drug substances were developed using GC-FID techniques. All the methods were validated according to the International Conference on Harmonization guidelines. The correlation coefficient values were found about 0.99. The obtained RSD values from the replicate injections in the range of 20 - 120% of the nominal concentration ensured the precision.

6

APPLICATION OF ION PAIR RP–HPLC METHOD IN PHARMACEUTICAL QUALITY CONTROL DISSOLUTION TESTING FOR SIMULTANEOUS ESTIMATION OF COMBINED TABLET DOSAGE FORMS WITH ACETYLSALICYLIC ACID AND GLYCINE

88%

Kowalska M. K. , Wozniak M. , Kijek M. , Krawczyk M. , Janas S.

Acta Poloniae Pharmaceutica - Drug Research

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2018

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tom 75

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nr 3

EN

The aim of the paper was to present the possibility of applying the novel method (RP-HPLC ion pair method) for the simultaneous dissolution determination of combined tablet dosage form containing acetylsalicylic acid and glycine in pharmaceutical industry. The samples were gradient eluted using a Pursuit XS Ultra C18 column (150x3.0 mm, with a particle size of 2.8µm) with variable composition of mobile phase A (1-heptanesulfonic acid sodium salt aqueous solution (2.8 g/L), pH 2.2 ± 0.05 adjusted with orthophosphoric acid) and phase B (methanol). The detection was carried out at 210 nm with a consist flow rate of 0.4 mL min−1. The method was validated by determining precision (repeatability and intermediate precision), accuracy, specificity, linearity, range, system suitability, robustness and stability in accordance with ICH guidelines. The method was accurate, precise and linear within the range of 0.03 – 0.18 mg mL−1 for acetylsalicylic acid and 0.016 – 0.096 mg mL−1 for glycine. The method is simple, convenient and suitable for analyzing acetylsalicylic acid and glycine in pharmaceutical formulations. The method could also be used for routine assay determination after small modification of sample preparation.

7

Method validation in quantitative electrochemical analysis of colchicine using glassy carbon electrode

88%

Bodoki E. , Săndulescu R. , Roman L.

Open Chemistry

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2007

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tom 5

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nr 3

766-778

EN

A cathodic differential pulse voltammetric determination of colchicine was validated using a glassy carbon electrode in HClO4/H3PO4 0.01 M. Colchicine gives an irreversible, diffusion-controlled peak at −862 mV vs. Ag/AgCl reference electrode. The cathodic peak is strongly influenced by a more alkaline environment with a shift towards more negative potentials. Method optimization was carried out in parallel for three types of electrodes (glassy carbon, mercury film and bismuth film coated glassy carbon). The cathodic peak current is higher using film-coated electrodes, but shows poorer intra-day reproducibility and a longer analysis time due to film renewal. Thus, a bare glassy carbon electrode was used to determine colchicine in the concentration range of 2.4 − 50 μg mL−1 (R 2 = 0.9998, n = 5), with a calculated detection limit of 0.80 μg mL−1. The proposed method was characterized according to ICH Harmonized Tripartite Guidance Q2(R1) by validation parameters (selectivity, linearity, accuracy, fidelity, limit of detection, limit of quantification) and it was successfully applied for the determination of colchicine from tablets, without the interference of the excipients. The method’s performances were evaluated and compared with both a known polarographic method and the official quantitative spectrophotometric determination from the Romanian Pharmacopoeia, Xth edition, respectively. [...]

8

METHOD VALIDATION AND STABILITY STUDIES OF DIFFERENTIAL ACTIVITY OF HYDROXYPROPYL-β-CYCLODEXTRIN AND HYDROPHILIC CARRIERS OF CARVEDILOL.

75%

Boakye-Yiadom K. O. , Kesse S. , Korto K. , Sarkodie E. K. , Baidoo S. A. , Filli M. S. , Wang B.

Acta Poloniae Pharmaceutica - Drug Research

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2020

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tom 77

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nr 3

423-430

EN

Stability studies of the formulations of CAR solid dispersions were analyzed at 300C/65%RH for a period of three months. A simple reverse phase HPLC was developed and validated for the quantification of CAR solid dispersions. Chromatographic separation was achieved on Waters Atlantis dC18 (4.6 X 150mm) column with a mobile phase consisting of 0.033M phosphate buffer and methanol (35:65). The mobile phase was filtered using an organic filter paper and sonicated for about 20 min. The flow rate was 1ml/min and 242nm wavelength was used for detection. Force degradation studies were conducted under three conditions namely; acidic, basic and hydroxide peroxide conditions. With the HPLC linearity concentration was in the range of 5-80μg/ml with a correlation coefficient (R2) of 0.9995. There was no interference with drug carriers. The suggested reverse phase HPLC methodology is simple, selective, linear and robust in quantifying the amount of CAR in the various solid dispersion samples. In hydrogen peroxide a degraded product was found on the chromatogram unlike that of the acidic and basic conditions. Degradation occurred more strongly in the acidic condition than in the basic condition. The binary systems were less stable than the ternary system solid dispersions due to the presence of HP-β-CD.

9

Jakość wyników pomiarów analitycznych problemy i wyzwania

63%

Konieczka P.

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2007

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tom Nr 56(607)

3-67

PL

W pracy przedstawiono główne problemy związane z oceną, kontrolą i zapewnieniem jakości wyników pomiarów analitycznych. Podano charakterystykę poszczególnych elementów systemu jakości wyników pomiarów analitycznych wraz z omówieniem aktualnego stanu wiedzy dotyczącego spójności pomiarowej. szacowania niepew-ności wyników pomiaru, walidacji procedur analitycznych, stosowania materiałów odniesienia oraz wykorzystania i interpretacji wyników badań międzylaboratoryjnych. W pierwszej części pracy przedstawiono definicję podstawowych pojęć związanych z systemem kontroli jakości wyników pomiarów analitycznych oraz opisano sposoby i metody ich wyznaczania. Druga część pracy dotyczy osiągnięć autora w dziedzinie określania i wyznaczania poszczególnych elementów systemu jakości. W zakresie wykorzystania i stosowania materiałów odniesienia opisano nową metodę otrzymywania bez matrycowego materiału odniesienia lotnych analitów, opartą na wykorzystaniu procesu termicznego rozkładu związków powierzchniowych. Przedstawiono także wyniki uzyskane przez autora w trakcie 2-letniego stażu naukowego w IRMM dotyczące udziału w procesie produkcji certylikowanych materiałów odniesienia (badania certyfikacyjne, badania trwałości materiałów). Przedstawiono także wstępne prace związane z produkcją laboratoryjnego materiału odniesienia. W zakresie walidacji metod analitycznych opisano wyniki wieloletnich prac autora związanych z opracowywaniem i definiowaniem nowych procedur analitycznych. Przedstawiono charakterystykę metody oznaczania zawartości fluorków w próbkach ciekłych z wykorzystaniem elektrody jonoselektywnej. Zaprezentowano metodę wykorzystującą technikę chromatografii gazowej w badaniach kinetyki reakcji hydrolizy [Beta]-laktamów - efekt rocznego stażu naukowego w Universidad del Pais Vasco w San Sebastian, Hiszpania. Przedstawiono także wyniki badań walidacyjnych metody oznaczania zawartości etanolu w preparatach farmaceutycznych opartych na wy-korzystaniu techniki HS-GC-FID. Opracowana metoda została wdrożona do praktyki analitycznej w Zakładach Farmaceutycznych POLPHARMA SA w Starogardzie Gdańskim. W zakresie badań między laboratoryjnych przedstawiono wyniki udziału autora w badaniach organizowanych przez CCQM, w trakcie jego 2-letniego stażu w IRMM. Opisano także sposób przeprowadzania porównań między laboratoryjnych współorganizowanych przez autora i opracowywania ich wyników. Opisano, zaproponowany przez autora pracy, prosty, zrozumiały i przejrzysty sposób opracowywania wyników badań międzylaboratoryjnych. Przedstawiono współzależności między poszczególnymi elementami systemu jakości wyników pomiarów analitycznych. Końcowym efektem zainteresowań naukowych autora jest zaproponowany i opisany zintegrowany system kontroli jakości wyników pomiarów, w którego skład wchodzą: - jasno zdefiniowany sposób szacowania niepewności wyników pomiarów analitycznych, - wykorzystujące podstawy metrologii i elementy statystyki matematycznej, przejrzyste sposoby wyznaczania wartości poszczególnych parametrów walidacyjnych, - opracowany jasny i prosty tok postępowania przy opracowywaniu wyników porównań międzylaboratoryjnych, ułatwiający uczestnikom badań interpretację otrzymanych wyników, - przedstawienie reguł towarzyszących wykorzystywaniu materiałów odniesienia.

EN

The main problems connected with quality assessment, quality control and quality management of analytical measurements are presented in the thesis. Characteristics of QA/QC system elements, together with the current stale of traceability, uncertainty estimation, method validation, CRM application and participation in PT are described. The first part of this treatise presents basic definitions from the QA/QC system and methods of their calculations. In the second part, the author presents his contribution to the field of determination and the calculation of particular QA/QC parameters. Within the frame of reference material production and its application, a new method for preparation of a matrix-free reference material of volatile analytes, based on thermal decomposition of surface compounds, is described. The results of studies obtained during 2-year postdocs fellows at IRMM connected with the certification and stability of CRMs are presented. Preliminary research related to the production of laboratory reference material is described. Results of the author's works related to scientific description and definition of new analytical procedures in the field of method validation are presented. The potentiometric method of determination of fluoride content in liquid samples by ion selective electrode is described. Application of GC in the investigation of kinetic of hydrolysis reaction of [Beta]-lactams as a result of a one-year fellowship at Universidad del Pais Vasco in San Sebastian, Spain are presented. Results of calculations for validation parameters for the HS-GC-FID method used for determination of ethanol content in pharmaceuticals are presented as well. This method has been applied in analytical practice in the Pharmaceutical Factory POLPHARMA SA in Starogard Gdański, in Poland Within the framework of interlaboratory comparison, the results of a proficiency test organized by CCQM, in which the author participated during a 2-year fellowship at IRMM, are presented. Organization and elaboration of PTs results are described. A simple, clear and comprehensible system of PTs result elaboration, suggested by the author, is presented. Interrelations among particular QA/QC system components are presented. The final effect of the author's interest is suggested and described, integrated into a QA/QC system, which consist of: - a clearly defined method for estimation of uncertainty of analytical results, - transparent methods for the determination of validation parameters, based on metrology and statistics, - a clear and simple procedure used for the elaboration of PTs results, which helps their participants interpret obtained results, - a presentation of rules connected with CRM production and application.

10

Stół słoneczny - projekt, budowa i walidacja metody pomiarowej

63%

Heim D. , Sipak A.

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2008

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tom z. 47 [252]

169-176

PL

Opisano zasadę działania, projekt oraz budowę stołu słonecznego zrealizowanego na Politechnice Łódzkiej w ramach pracy dyplomowej. Dokonano przeglądu istniejących rozwiązań stołów słonecznych oraz omówiono wady i zalety ich wykorzystania dla potrzeb wyznaczania oddziaływania promieniowania bezpośredniego na obiekty architektoniczne. Określono przyjęte założenia oraz sposób walidacji urządzenia i metody pomiarowej dla potrzeb działalności naukowo-dydaktycznej. Na koniec zaprezentowano przykłady aplikacji i symulacji światła słonecznego przy pomocy omawianego urządzenia.

EN

This paper described original project of Artificial Sun developed at Technical University of Łódź. The construction type, realisation process as well as validation method was presented and discussed. This laboratory stand was realized individually by Artur Sipak MSc student.

11

Stability-indicating LC method for determination of tadalafil in bulk drug and pharmaceutical dosage form

63%

Mathpati M. M. , Sangshetti J. N. , Rane V. P. , Patil K. R. , Shinde D. B.

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2009

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tom Vol. 54, No. 4

679-689

EN

A novel stability-indicating LC assay method for quantitative determination oftadalafil in bulk drug and pharmaceutical dosage form in the presence of forced-degradation products was developed and validated. An isocratic reversed phase LC method was developed to separate the drug from its degradation products using a Zorbax SB-C18 column and water-acetonitrile mixture as a mobile phase. Detection was carried out at the wavelength of 235 nm. Tadalafil was subjected to stress conditions in order to perform its hydrolytic (acid, base), oxidative, photolytic, and thermal degradation. Degradation oftadalafil was observed in the presence of acid, base, and 30% H2O2. The drug was found to be stable under other stress conditions. The signals of degradation products were well-resolved from the main peak oftadalafil. Percentage recovery oftadalafil in pharmaceutical dosage form ranged from 98.89% to 101.25%. The developed method was validated with respect to linearity, accuracy (recovery), precision, specificity, and robustness. Forced degradation studies proved the stability-indicating power of the method.

PL

Opracowano i zwalidowano nową metodę ilościowego oznaczania tadalafilu za pomocą chromatografii cieczowej, w obecności produktów rozkładu, pozwalającą na ocenę stabilności surowca i formy farmaceutycznej. Zastosowanie kolumny Zorbax SB-C18 i izokratycznej mieszaniny woda —acetonitryl pozwalało na rozdzielenie leku od produktów rozkładu. Detekcję przeprowadzono przy długości fali 235 nm. Tadalafil poddano ekstremalnym warunkom w celu uzyskania hydrolitycznych (kwas, zasada), oksydatywnych. tbtolitycznych i termicznych produktów rozkładu. Rozkład tadalafilu obserowwoano w obecności kwasów, zasad i 30% H,O2. Lek okazał się trwały w pozostałych ekstremalnych warunkach. Sygnały produktów rozkładu były dobrze oddzielone od głównego piku tadalafilu. Odzysk w przypadku badania postaci farmaceutycznej wynosił od 98,89% do 10 l ,25%. Opacowana. metodę zwalidowano w zakresie liniowości, dokładności (odzysku), precyzji, specyficzności i odporności na zmiany warunków otoczenia. Badania rozkładu w warunkach ekstremalnych wykazały przydatność opracowanej metody do oceny stabilności leku.