Catalogo dei Corsi di studio

General objectives
The course aims to provide students with the theoretical and practical knowledge related to drug dosage; in addition, the course provides information on the pharmaceutical and toxicological properties of drugs
Specific objectives
1. Knowledge and understanding
The student will be able to use the method of analysis proposed by the FU, for the dosing of a drug. Furthermore it will be able to treat the sample to be subjected, depending on the pharmaceutical form. He will also be able to use the instruments used in the quantitative laboratory.
2. Ability to apply knowledge and understanding
At the end of the course, the student will be able to analyze the sample consisting of an active ingredient contained in a drug by selecting the most suitable method to obtain reproducible results. To this end, knowledge of the chemical structure and reactivity of organic molecules will be fundamental for the selection of the method itself (analysis based on acid-base reactions; analysis based on redox reactions; analysis based on the formation of a precipitate; analysis based on the formation of complex); The experience of practical laboratory exercises will allow the student to learn to apply and observe what has already been discussed during the lectures. The knowledge of the properties and reactivity of organic substances will allow the student not only to understand the functions of biological, pharmacological and toxicological interest expressed by these substances, but also to design and / or identify possible approaches for the resolution of related problems. The knowledge of the most widespread diseases together with the knowledge of drugs, from a pharmacological, therapeutic and toxicological point of view, will make the student skilled and intuitive in the rational choice / advice of these drugs in the field of human health.
3. Autonomy of judgment
The teacher will stimulate students to develop the logical-critical sense by giving interactive lessons, through frequent questions during the lesson, with the aim of inducing them to acquire the ability to connect the various concepts defined in the program, of mastery of the subject, but also to consider the study of the analysis of Medicinal II as an integral part of other disciplines already studied (general and inorganic chemistry, organic chemistry, biochemistry, and the analytics acquired in previous years). The teacher periodically proposes to the students of the days defined "question time" in which some students will ask for clarifications about the topics treated previously and other students will try to give the answer, in this way a contradictory is created, among the students, at the end of which the teacher will re-explain the topics that are less clear or in any case those solicited by the students. At the end of the course the students will be able to formulate an analytical / critical judgment, interpret and correlate complex concepts, design a research concerning the topics covered in order to broaden scientific, ethical and social knowledge.
4. Communication skills
Through the acquisition of knowledge and understanding, of the ability to apply them and to propose a critical judgment on the topics dealt with, but also through the use of the relative scientific language used by the teacher during the course and the frequent stimulation to the communication of what was learned in lesson, the student will be able to communicate with cognitive and linguistic-perceptive depth with his / her peers and / or belonging to an inherent scientific and social community or of different cultural background.
5. Learning skills
The student who has acquired the abilities described above may be able to undertake future studies in a more autonomous, self-managed and rapid manner, but also to propose thematic social and / or work contexts useful to the scientific progress of society in the field of human health.

Programme

General part (6h) - Safety in the workplace, current legislation. Safety in educational laboratories. The Official Pharmacopoeia, the National Formulary, Codex. Definition of drug. Classification of analytical methods: qualitative and quantitative. Analysis of a pharmaceutical preparation: sampling, choice of the method of analysis, evaluation of the results obtained.
Instrumentation required in quantitative analysis: calibrated and graduated glassware, analytical and technical balance. Scale characteristics, weighing operations;
Definition of: average, median, precision and accuracy. Certain and indeterminate errors. Certain errors: revelation of effects and correction. Indeterminate errors: statistical treatment. Properties of the normal error curve, mean deviation, standard deviation. abnormal value deviation, 4d rule, 2.5d rule, Q rule
Gravimetric analysis (6h)
Theoretical aspects of precipitation; weighted determinations without transformation of the sample, weighted determinations with transformation of the sample, precipitation of a compound in the homogeneous phase, coprecipitation, glassware in use in the gravimetric analysis ;. Weight determination of a precipitate: precipitation, digestion, filtration, washing, drying and calcination, gravimetric factor.
Volumetric analysis (40 h)
Generality; Types of reactions used in volumetric analysis; equivalent point; titration curves - construction of a strong-base strong acid titration curve; weak-strong acid base and vice versa; salts. Ways of expressing concentrations; pH calculation; buffer solutions; acid base indicators.
Acidimetry: the mother substances; preparation and standardization of a HCl solution, choice of indicator. Applications: sodium carbonate determination, alkaline mixtures - Winkler method and Warder method; determination of ammoniacal nitrogen: distillation method;
Alkalimetry: the mother substances; preparation and standardization of a sodium hydroxide solution. Applications: determination of acetyl salicylic acid; determination of boric acid; determination of citric acid; determination of phosphoric acid; borax determination; determination of chloral hydrate;
Precipitation formation titration: Mohr, Vohlard, Fajans method. Applications: preparation and standardization of a silver nitrate solution; preparation and standardization of a thiocyanate solution. Cyclophosphamide; Clorbutanolo; Chloral hydrate; Mercuric iodide; mercury; Mercury yellow oxide; merbromin;
Complexometry and chelometry: generalities;
Chelometry: EDTA, α and β factors; final point: instrumental method, chromic metal indicators. Chelometric titrations: direct, inverse, by displacement. Masking. Applications: preparation and standardization of an EDTA solution. Aluminum determination; determination of football; magnesium determination; mercury determination; zinc determination; determination of water hardness.
Redox titrations: general, electrode potential, formal potential. Redox indicators.
Applications: Cerimetry: menadione, paracetamol. Permanganometry: preparation and standardization of a permanganate solution; determination of calcium, iron, hydrogen peroxide.
Iodimetry and iodometry: generalities; influence of pH on equilibria; preparation and standardization of an iodine solution; preparation and standardization of a thiosulphate solution; iodimetry applications: ascorbic acid determination; determination of carbasone; determination of dimercaprol; mercurous chloride determination; determination of sodium thiosulfate. Iodometry application: active chlorine determination in hypochlorites; hydrogen peroxide determination; chloramine determination; Bromometry: phenol determination; isoniazid determination; sobrerolo determination.
Titration in non-aqueous solvent (5h)
Generality; Solvents and their characteristics: aprotic, protophilic, protogenic, amphiprotic; the indicators. Base titrations: preparation of a solution of perchloric acid; FU applications; Acid titrations: preparation of a solution of tetrabutylammonium hydroxide (TBA); FU applications; titrations of salts.
Instrumental analysis (20h)
Potentiometric analysis: general; reference electrodes and indicator electrodes; glass electrode. Conductimetry: general concepts; conductivity measurements: the Wheastone bridge and the Kohlraush bridge. Kirchoff's law; Conductometric titrations: strong strong base acid; weak acid strong base: Kolthoff method, Davien-Righellato method; Davien method.
Optical analysis methods: interaction between molecules and radiant energy; atomic spectra and molecular spectra; the law of Lambert and Beer, deviations; absorption spectra - methods of analysis: direct, by comparison; UV-Vis and IR spectrophotometry; UV-Vis spectra HOMO-LUMO transitions; absorption bands and factors that influence bandwidth; infrared spectrophotometry: theory; absorption bands of some functional groups. The IR spectrum.
Chromatographic analysis methods: general concepts; the separative process; chromatographic methods; Quantitative HPLC analysis.

Adopted texts

G. C. Porretta Analisi di preparazioni farmaceutiche – Analisi Quantitativa – Ed CISU

Bibliography

Testi di consultazione: Skoog, West, Holler, Fondamenti di Chimica Analitica, Ed Edises R. Cozzi, P. Protti, T. Ruaro. Analisi Chimica Strumentale. A. Metodi Elettrochimici, Zanichelli Bologna R. Cozzi, P. Protti, T. Ruaro. Analisi Chimica Strumentale. A. Metodi Ottici, Zanichelli Bologna

Prerequisites

The Medicinal Analysis II course is at the 4th year of the Pharmacy course; it is clear that the knowledge required of the student is of a biological and chemical type; in particular, by treating the course of drug analysis, the student, in order to understand the analytical techniques and then apply them will need to know the drug and therefore require knowledge of pharmaceutical chemistry and will also have knowledge of inorganic and organic chemistry.

Frequency modes

Course attendance is mandatory; for lectures it is advisable to attend but 70% of the lessons are considered valid: as far as practical exercises are concerned, absences are not allowed, except for serious reasons, which in any case must be recovered. The practical course is developed in two ways: a compulsory basic course for all students of 8-10 exercises and an advanced course which will be optional (8-10 additional exercises).

Exam modes

Students are assessed mainly through an oral test in which the learning of the subject and the mastery that the student has acquired will be verified, using examples that require some calculations; the final vote will also take into account the final practical test.

Exam reservation date start	Exam reservation date end	Exam date
01/02/2020	13/02/2020	17/02/2020
15/04/2020	29/04/2020	05/05/2020
06/05/2020	18/05/2020	25/05/2020
25/05/2020	05/06/2020	15/06/2020
20/06/2020	30/06/2020	13/07/2020
25/08/2020	10/09/2020	21/09/2020
01/11/2020	15/11/2020	23/11/2020
25/11/2020	04/12/2020	14/12/2020
01/01/2021	15/01/2021	25/01/2021

Programme

Purposes of quantitative analytical chemistry. Fields of application of quantitative pharmaceutical analysis. Contamination of drugs. F.U. XII ed. and Ph.Eur. IX. Stages of a quantitative analysis: choice of method, sampling, sample preparation, replicates, solubilization, interferences. Scale of analyzes. Units of measurement and expressions of concentration. 4 hours

Evaluation of analytical data. Average, median, precision, accuracy, deviation, error. Systematic errors. Identification and elimination of instrumental, personal and method errors. Constant and proportional systematic errors - Random errors. Significant figures. 2 hours

Gravimetric analysis:
Analytical scale. Mass and weight, two-plate scales, one-plate scales, weighing methods. Electronic scale. Weighing errors. Stoichiometry: gravimetric factor. Solubility and solubility product. Factors influencing the solubility of a precipitate: common ion, pH, complex ion formation, electrolyte concentration, temperature and solvents. Separations based on the difference in solubility. Precipitation process: mechanism of formation of a precipitate, colloidal precipitates, crystalline precipitates, adsorption, flocculation, peptization, digestion, filterability. Contamination of precipitates: co-precipitation, post-precipitation. Precipitation in homogeneous phase. Organic precipitants: chelate complexes, ionic combination compounds. Phases of a gravimetric analysis: preliminary treatments, precipitation, digestion, filtration, washing, drying, calcination. Applications: determination of SO4 =, Ba ++, Fe + 3, Al + 3. 4 hours

Volumetric analysis:
Standard solutions, primary standards, equivalence point, end point, titration error. Stoichiometry: definition of equivalent weight for neutralization, oxidation-reduction, precipitation and complex formation reactions. Concentration expressions used in volumetric calculations (normality, title Determination of the end point, titration curves and choice of the indicator Equipment used in the volumetric analysis. 2 hours

a) Neutralization:
Titrations Acid-base definitions, pH calculation, indicators. Titration curves of acids and strong bases, of weak acids and bases; dependence of the titration curves from the concentration and dissociation constants. Titration curves of polyprotic acids. Titration of mixtures of strong and weak acids. Preparation of standard solutions of acids or strong bases. Effect of CO2 on standard base solutions. Determination of alkaline mixtures. Kjeldhal method for the determination of nitrogen in organic substances, determination of ammonium salts, nitrates and nitrites. Determination of ammonium salts using the formaldehyde method. Determination of boric acid and borax. Determination of organic substances, direct and indirect methods: determination of carboxylic acids, sulfonic acids, amines, esters, aldehydes and ketones, alcohols. Titrations in non-aqueous environment. 18 hours


b) Precipitation titrations:
Argentometric. Titration curves and factors influencing them. Indicators. Method of Mohr, of Volhard, of Fajans. Applications: preparation of standard solutions of AgNO3, NH4SCN. Determination of chloral hydrate, amidotrizoic acid, cyclophosphamide and proteinate silver. 6 hours

c) Complexometric titrations:
Ligandi, constant formation of a complex. Titration curves. Titrations with monodentate ligands: determination of cyanides according to Liebig. Titrations with chelators: EDTA, composition of EDTA solutions as a function of pH, complexes between EDTA and metal ions. Effect of pH on the titration curves (actual formation constant, factor ). Effect of auxiliary complexing agents on the titration curve (actual formation constant, factor ). Determination of the end point: metallochromic indicators. Titration methods: direct titration, retrotitulation, titration by displacement, indirect titration. Masking. Determination of Mg ++, Ca ++, water hardness. 8 hours

d) Oxide-reduction titrations:
Oxidation state of organic compounds. Titration curves of Fe ++ with Ce + 4, MnO4-. Dependence of titration curves from concentration and equilibrium constant. Determination of the end point: oxidation-reduction indicators.
Permanganometry. Reactions of KMnO4 in acidic, neutral and alkaline environment. Preparation of a standard solution of KMnO4, primary standards, determination of the end point. Applications: determination of Ca ++, Fe ++ (pre-production of Fe + 3 with the Jones reducer and with SnCl2), H2O2.
Cerimetry. Features, advantages and disadvantages. Preparation of a standard Ce (IV) solution. Determination of ferrous gluconate, paracetamol and menadione.
Iodimetry and Iodometry. Determination of the end point, influence of pH. Iodimetry: preparation of a standard iodine solution, determination of the potassium tartrate antimony, Vitamin C; Karl Fischer method for water determination: reactions, amperometric titration and method limits. Iodometry: preparation of a standard sodium thiosulphate solution, determination of chloramine T, hypochlorite and H2O2.
Bromometria. Preparations of standard solutions of Br2. Indirect methods: determination of aromatic organic compounds (applications: determination of phenols). Direct methods: sobrerol determination. 18 hours

Potentiometry Equipment. Reference electrodes. Metal indicator electrodes of first, second, third species and redox. Membrane electrodes. Classification of membranes. Properties of ion-selective membranes. Glass electrode for pH measurement: composition, structure, hygroscopic character and conductivity. Alkaline error. Potentiometric measurements of pH with glass electrode. Potentiometric titrations.
Spectroscopic methods of analysis. Wavelike and particle properties of light. Electromagnetic spectrum. Optical spectroscopy: materials, sources, detectors. Wavelength selection devices: absorption and interference filters; lattice monochromators. Single and double-beam instruments. Absorption theory. Atomic and molecular absorption. Beer's law. Apparent and real limits. Procedural details: selection of the wavelength; variables that influence absorbance; cleaning and handling of cells; determination of the relationship between absorbance and concentration; method of the standard addition. Spectrophotometric titrations. 10 hours

Adopted texts

Skoog, West, Holler: “Chimica Analitica - Una Introduzione” EdiSES

G.C. Porretta: “Analisi di Preparazioni Farmaceutiche - Analisi Quantitativa” Ed. CISU

Prerequisites

The Medicinal Analysis II course is at the 4th year of the Pharmacy course; it is clear that the knowledge required of the student is of a biological and chemical type; in particular, by treating the course of drug analysis, the student, in order to understand the analytical techniques and then apply them will need to know the drug and therefore require knowledge of pharmaceutical chemistry and will also have knowledge of inorganic and organic chemistry. Necessary for the understanding of the lessons the concepts of: General and Inorganic Chemistry, Organic Chemistry, Analytical Chemistry and Complements of General and Inorganic Chemistry. Important the acquisition of knowledge on: Medicinal Chemistry I, Pharmaceutical and toxicological chemical analysis, Medicinal Analysis I. Useful to have acquired notions of Mathematics.

Exam modes

The assessment method of the course is characterized by exam session according to a calendar proposed at the beginning of the academic year. The exam consists of a written test and an oral test. The written exam lasts an average of two hours; the oral exam lasts an average of one hour; during this timespan the teacher examines the candidate on his knowledge of all the subjects. Topics must be displayed in a appropriate language, using appropriate terms.
The elements taken into consideration for the evaluation are: knowledge of the subjects, the use of an appropriate language, the active participation during the lectures, the ability of reasoning demonstrated during the trial, the ability to study autonomously on the texts.
Sufficient knowledge of the topics is required for passing the exam with minimum grades. To achieve a score of 30/30 cum laude, the student must demonstrate have acquired excellent knowledge of all the topics covered during the course, being able to link them in a logical and consistent way. The student must also be able to draw up original results based on the knowledge acquired.

Exam reservation date start	Exam reservation date end	Exam date
06/01/2020	16/01/2020	20/01/2020
01/02/2020	16/02/2020	17/02/2020
05/05/2020	17/05/2020	22/05/2020
01/06/2020	10/06/2020	16/06/2020
12/06/2020	23/06/2020	03/07/2020
05/09/2020	15/09/2020	21/09/2020
23/10/2020	05/11/2020	10/11/2020
20/11/2020	28/11/2020	01/12/2020
01/01/2021	14/01/2021	19/01/2021