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Use of liquid chromatography in pharmaceutical analysis and preparation of monolithic stationary phases for thin-layer chromatography
Vojta, Jiří
(EN) In the first part of this work, analytical methods for determination of impurities of active pharmaceutical ingredients (API) in combined pharmaceutical dosage forms were developed and validated. Development of the methods covered both the optimization of sample preparation procedure and chromatographic conditions. The methods were validated according to International Conference on Harmonization guideline and both of them were confirmed to be able to analyze stability samples. Impurities in paracetamol, codeine phosphate hemihydrate and pitophenone hydrochloride in the presence of fourth API fenpiverinium bromide were separated by using ion-pair reversed phase chromatography with gradient elution. Symmetry C18, 250 x 4,6 mm, 5 µm heated to 35 řC was used as a separation column. A diode array detector was used. The detection wavelengths were set as follows: 220 nm for paracetamol impurity K, 245 nm for paracetamol and its other impurities and 285 nm for codeine, pitophenone and their impurities. Impurities in valsartan, amlodipine besylate and hydrochlorothiazide were separated by reversed phase UHPLC method with gradient elution. Chromatographic column Zorbax Eclipse C8 RRHD, 100 x 3,0 mm, 1,8 µm heated to 30 řC and spectrophotometric detection were used. The detection wavelengths were set as...
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Determination of Paracetamol content in selected drugs using ATR-FTIR spectrometry
Waczulíková, Kristína ; Sedláček, Petr (referee) ; Enev, Vojtěch (advisor)
This bachelor thesis deals with determination of paracetamol content in selected drugs by ATR-FTIR spectrometry and aims to design and optimize determination of paracetamol in dosage forms by a direct measurement of the sample, called ‘dry way’. Tablets of three drugs containing paracetamol have been studied. Wavelength ranges were determined from the measured FTIR spectra as regions where the absorptions of fillers (microcrystal cellulose, starch and magnesium stearate) were minimal. Absorption bands of paracetamol were selected at the wavenumbers of 1 503 cm-1 and 1 224 cm-1 in order to construct a calibration curve. The contents of paracetamol in the drug tablets were calculated using calibration curves obtained by the method of simple regression analysis. The lowest deviation from the amount of 500 mg paracetamol per tablet as reported by the manufacturer was from the calibration curve for paracetamol with microcrystalline cellulose. The determined amounts of paracetamol per tablet in the selected drugs lied within range 493.5–505.5 mg. These results point to the conclusion that the ATR-FTIR spectrometry method can be used for the quantitative determination of paracetamol in drugs using direct measurement, as deviations from the reference value of 500 mg did not exceed 1.5 % for cellulose and 3.85 % for magnesium stearate and therefore are within acceptable limits for the exploratory study.
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Adsorption of pharmaceuticals from aqueous solutions onto clay minerals
Vallová, S. ; Sokolová, B. ; Valovičová, Věra ; Plevová, Eva
The objective of this work was to investigate to possibility of clay minerals for the removal of drugs from aqueous solutions. Natural minerals such as montmorillonite, vermiculite, kaolinite and modified montmorillonites KSF and K10 (intercalated by Fe3+) were used as potential sorbents for three analgetics: paracetamol, ibuprofen and diclofenac from aqueous solutions. This research demonstrated that adsorption of all three pharmaceuticals onto natural untreated clay minerals, except paracetamol sorption on Na-MMT, is negligible. On the other hand, the chemically modified montmorillonites demonstrated significant sorption ability in the order diclofenac>ibuprofen>paracetamol.
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Analysis of sellected drugs with the use of TLC as a topic of laboratory courses
Menzel, Petr ; Kolář, Karel (advisor) ; Rusek, Martin (referee)
The paper aims to mediate thin film chromatography analysis by means of drugs commonly found in households (analgesic-antipyretics) to secondary school and grammar students, or to college students. For this purpose, laboratory tasks have been designed to cover all levels of the Bloom pyramid so that the educational potential is as high as possible. This is closely related to the topic of drug expiration and treatment. Pupils and students should take on both the competences of knowledge, skills, and attitudes. Keywords: thin layer chromatography; TLC; chromatography in education; educational experiment; expiratory medication; drug handling; analgesic- antipyretics, acetylsalicylic acid, paracetamol
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Pharmacotherapy of headaches in adults
Holinská, Eliška ; Hrdina, Radomír (advisor) ; Tilšer, Ivan (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Pharmacology and Toxicology Student: Eliška Holinská Supervisor: Prof. MUDr. Radomír Hrdina, CSc. Title of diploma thesis: Pharmacoteraphy of headache in adults Headache is one of the most common health problem that encounters almost everyone during the life. Depending on the cause, headaches can be divided on the primary headaches, which are the subject of the diploma thesis, and secondary headaches, which are caused by other diseases. The primary headaches are migraine, tension-type headache, cluster headache and primary chronic daily headache. Headache is not a life-threating condition but it can significantly reduce the quality of life, particularly the chronic forms of headache. The determination of the right diagnosis is essential for the choice of appropriate therapy. For primary headache are typical negative test results, there are no structural lesions or signs of organic brain damage. Diagnostics is comlicated and it is primarily based on a carefully processed medical history. In the therapy of primary headache are used both pharmacological and non-pharmacological methods, optimaly in combination. Pharmacological treatment consists of preventive and acute therapy. The preventive treatment is given to reduce the...
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Use of liquid chromatography in pharmaceutical analysis and preparation of monolithic stationary phases for thin-layer chromatography
Vojta, Jiří ; Coufal, Pavel (advisor) ; Tůma, Petr (referee) ; Jelínek, Ivan (referee)
(EN) In the first part of this work, analytical methods for determination of impurities of active pharmaceutical ingredients (API) in combined pharmaceutical dosage forms were developed and validated. Development of the methods covered both the optimization of sample preparation procedure and chromatographic conditions. The methods were validated according to International Conference on Harmonization guideline and both of them were confirmed to be able to analyze stability samples. Impurities in paracetamol, codeine phosphate hemihydrate and pitophenone hydrochloride in the presence of fourth API fenpiverinium bromide were separated by using ion-pair reversed phase chromatography with gradient elution. Symmetry C18, 250 x 4,6 mm, 5 µm heated to 35 řC was used as a separation column. A diode array detector was used. The detection wavelengths were set as follows: 220 nm for paracetamol impurity K, 245 nm for paracetamol and its other impurities and 285 nm for codeine, pitophenone and their impurities. Impurities in valsartan, amlodipine besylate and hydrochlorothiazide were separated by reversed phase UHPLC method with gradient elution. Chromatographic column Zorbax Eclipse C8 RRHD, 100 x 3,0 mm, 1,8 µm heated to 30 řC and spectrophotometric detection were used. The detection wavelengths were set as...
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Use of liquid chromatography in pharmaceutical analysis and preparation of monolithic stationary phases for thin-layer chromatography
Vojta, Jiří
(EN) In the first part of this work, analytical methods for determination of impurities of active pharmaceutical ingredients (API) in combined pharmaceutical dosage forms were developed and validated. Development of the methods covered both the optimization of sample preparation procedure and chromatographic conditions. The methods were validated according to International Conference on Harmonization guideline and both of them were confirmed to be able to analyze stability samples. Impurities in paracetamol, codeine phosphate hemihydrate and pitophenone hydrochloride in the presence of fourth API fenpiverinium bromide were separated by using ion-pair reversed phase chromatography with gradient elution. Symmetry C18, 250 x 4,6 mm, 5 µm heated to 35 řC was used as a separation column. A diode array detector was used. The detection wavelengths were set as follows: 220 nm for paracetamol impurity K, 245 nm for paracetamol and its other impurities and 285 nm for codeine, pitophenone and their impurities. Impurities in valsartan, amlodipine besylate and hydrochlorothiazide were separated by reversed phase UHPLC method with gradient elution. Chromatographic column Zorbax Eclipse C8 RRHD, 100 x 3,0 mm, 1,8 µm heated to 30 řC and spectrophotometric detection were used. The detection wavelengths were set as...
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Pharmacovigilance in the Toxicological Information Centre
Urban, Michal ; Pelclová, Daniela (advisor) ; Benešová, Veronika (referee) ; Zacharov, Sergej (referee)
1 ABSTRACT Background The annual drug overdose rates have been increasing exponentially since the 90's worldwide. Toxicological information centre (TIC) represents a valuable source of information for evaluating the trends in the drug poisonings in Czech Republic. Aim of the study The purpose was to analyze the number and trends in the calls concerning poisonings due to central nervous system (CNS) affecting drugs, identify the reasons of medication errors caused by laymen, frequency and consequences of these errors across all age groups and also to analyze the numbers, causes, symptoms and severity of the paracetamol intoxications. Methods During the reference period the data from the enquiries were extracted from the TIC electronic database, discharge reports from the hospital were studied or phone call follow-ups with the patients were carried out to be able to evaluate the outcome of the poisonings. Results In the years 1997-2002 the number of calls caused by poisoning with tricyclic antidepressants and barbiturates decreased (by 366.7 % and 340,0 %, respectively) whereas the calls due to selective serotonin reuptake inhibitors and benzodiazepines overdose increased (by 1347.4 % and 359.8 %). The 0-5 years old children are at the highest risk of experiencing medication errors or accidental poisonings...
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