Eduardo Maria SOMMELLA | PHARMACEUTICAL ANALYSIS I
Eduardo Maria SOMMELLA PHARMACEUTICAL ANALYSIS I
cod. 0760400009
PHARMACEUTICAL ANALYSIS I
| 0760400009 | |
| DIPARTIMENTO DI FARMACIA | |
| EQF7 | |
| PHARMACEUTICAL CHEMISTRY AND TECHNOLOGY | |
| 2024/2025 |
| OBBLIGATORIO | |
| YEAR OF COURSE 2 | |
| YEAR OF DIDACTIC SYSTEM 2023 | |
| AUTUMN SEMESTER |
| SSD | CFU | HOURS | ACTIVITY | |
|---|---|---|---|---|
| CHIM/08 | 6 | 48 | LESSONS | |
| CHIM/08 | 4 | 48 | LAB |
| Objectives | |
|---|---|
| THE COURSE AIMS TO PROVIDE THE STUDENT WITH THE THEORETICAL, PRACTICAL AND METHODOLOGICAL CONCEPTS TO PERFORM THE QUANTITATIVE ANALYSIS OF MOLECULES OF PHARMACEUTICAL, NUTRACEUTICAL AND COSMECEUTICAL INTEREST THROUGH CLASSICAL AND ADVANCED/INSTRUMENTAL ANALYSIS APPROACHES DESCRIBED IN THE MAIN PHARMACOPOEIAS. KNOWLEDGE AND UNDERSTANDING THE THEORETICAL PRINCIPLES CONCERNING THE PURIFICATION AND QUANTITATIVE ANALYSIS METHODS OF APIS (ACTIVE PHARMACEUTICAL INGREDIENTS) WITH PARTICULAR REGARD TO THOSE REPORTED IN THE PHARMACOPOEIAS. CALCULATION APPROACHES FOR SOLVING EXERCISES CONCERNING THE DOSAGES OF MOLECULES OF PHARMACEUTICAL INTEREST. THE PRACTICAL, METHODOLOGICAL, AND INSTRUMENTAL ASPECTS TO BE PERFORMED IN THE CHEMICAL-PHARMACEUTICAL LABORATORY FOR THE QUANTITATIVE DETERMINATION BY MEANS OF SEPARATION TECHNIQUES, PURIFICATION OF MOLECULES OF PHARMACEUTICAL INTEREST. APPLYING KNOWLEDGE AND UNDERSTANDING - DESCRIBE THE THEORETICAL AND PRACTICAL ASPECTS OF CLASSICAL AND ADVANCED CHEMICAL-PHARMACEUTICAL ANALYSIS METHODS - QUANTITATIVELY ANALYZE MOLECULES OF PHARMACEUTICAL INTEREST USING CLASSICAL, INSTRUMENTAL (CHROMATOGRAPHIC/SPECTROSCOPIC) TECHNIQUES - PROCESS THE OBTAINED QUANTITATIVE DATA IN A STATISTICALLY CRITICAL WAY AND EVALUATE THEIR VALIDITY - SOLVING CALCULATION EXERCISES RELATED TO THE DOSAGE OF MIXTURES OF MOLECULES OF PHARMACEUTICAL AND/OR NUTRACEUTICAL/COSMECEUTICAL INTEREST MAKING JUDGMENTS - EVALUATE THE PROCEDURES USED WITH A CRITICAL SENSE, THROUGH THE USE OF CALCULATIONS, STATISTICAL APPROACHES AND RESULTS VALIDATION - DESIGN PROTOCOLS FOR THE QUANTITATIVE DETERMINATION OF APIS AND IMPURITIES DESCRIBED IN THE MAIN PHARMACOPOEIAS - SELECT THE MOST APPROPRIATE METHODS FOR THE PURIFICATION, SEPARATION AND QUANTITATIVE DETERMINATION OF MOLECULES OF PHARMACEUTICAL INTEREST COMMUNICATION SKILLS COMMUNICATE AND PRESENT BY MEANS OF REPORTS ALSO IN DIGITAL FORMAT, AND IN A MULTIDISCIPLINARY CONTEXT, THE RESULTS OF THE MOST SUITABLE PROTOCOLS FOR SOLVING PROBLEMS RELATED TO THE QUANTITATIVE DETERMINATION OF MOLECULES OF PHARMACEUTICAL, NUTRACEUTICAL AND COSMECEUTICAL INTEREST ABILITY TO LEARN - USE THE TOOLS ACQUIRED FOR THE CRITICAL EVALUATION OF TEXTS SUCH AS PHARMACOPOEIA MONOGRAPHS, OR CERTIFIED OR DESCRIBED IN THE LITERATURE ANALYSIS METHODS FOR THE QUANTITATIVE DETERMINATION OF APIS AND IMPURITIES AND THE SELECTION, IN THE CONTEXT OF PROBLEM SOLVING, OF DIFFERENT POSSIBLE SOLUTIONS |
| Prerequisites | |
|---|---|
| THE ACQUISITION OF OBJECTIVES RELATED TO THE FOLLOWING DISCIPLINES IS REQUIRED: GENERAL AND INORGANIC CHEMISTRY, PHYSICS, MATHEMATICS, AND THE ACQUISITION OF ANALYTICAL CHEMISTRY OBJECTIVES AND A BASIC KNOWLEDGE OF ENGLISH AND COMPUTER TECHNOLOGY IS STRONGLY RECOMMENDED. |
| Contents | |
|---|---|
| THEORY INTRODUCTION TO QUANTITATIVE ANALYTICAL CHEMISTRY, LABORATORY OPERATIONS, SAFETY IN LABORATORY, OFFICIAL ITALIAN PHARMACOPOEIA (F.U.). THE EUROPEAN PHARMACOPOEIA (E.P.). GLASSWARE AND ITS USE. ELECTRONIC SCALES. HOW TO EXPRESS A RESULT: NUMERICAL VALUE, UNCERTAINTY, UNIT OF MEASUREMENT, WORKING SCALES SUMMARY OF THE THEORY OF ERRORS. CONCENTRATION UNIT. MOLARITY, NORMALITY, EQUIVALENTS. (4 H, 0.50 CFU) VOLUMETRIC ANALYSIS. PH CALCULATION OF STRONG AND WEAK ACIDS AND BASES. PH CALCULATION OF POLYPROTIC ACIDS AND BASES AND THEIR SALTS. TITRATION CURVES OF ACIDS AND BASES. INDICATOR THEORY. MAIN ACID-BASE INDICATORS AND THEIR USE. PRIMARY AND SECONDARY STANDARDS, CHARACTERISTICS AND THEIR USE. STANDARD SOLUTIONS OF ACIDS AND BASES USED IN VOLUMETRIC ANALYSIS. EXAMPLES OF ACIDIMETRIC AND ALKAMETRIC DETERMINATIONS (10 H, 1,25 CFU) GRAVIMETRY. SOLUBILITY. SOLUBILITY PRODUCT. PRECIPITATION AND REDISSOLUTION OF PRECIPITATES. COLLOIDAL AND CRYSTALLINE PRECIPITATES. RELATIVE OVERSATURATION. PRECIPITATION TITRATION CURVES, DETERMINATION OF HALIDES ACCORDING TO MOHR, VOLHARD, FAJANS AND LIEBIG-DENIGES. PREPARATION OF STANDARD SOLUTIONS USED IN PRECIPITOMETRY. EXAMPLES OF PRECIPITOMETRIC DETERMINATIONS ACCORDING TO E.P. (8 H, 1 CFU) COMPLEX METRIC TITRATION. METALLOCHROMIC INDICATORS. CONSTANTS OF EQUILIBRIUM AND STABILITY OF COMPLEXES. PREPARATION OF STANDARD SOLUTIONS USED IN COMPLEXOMETRY. EXAMPLES OF COMPLEXOMETRIC DETERMINATIONS ACCORDING TO E.P. (2 H, 0.25 CFU) OXIDOMETRY: DEFINITION AND USE OF THE STANDARD REDUCTION POTENTIAL. REDOX INDICATORS AND SPECIFIC INDICATORS. PERMANGANOMETRY. IODIMETRY. IODOMETRY. CERIMETRIC. BROMOMETRY. PREPARATION OF STANDARD SOLUTIONS USED IN REDOX TITRATION. EXAMPLES OF REDOX DETERMINATIONS ACCORDING TO E.P. ELECTRODES AND PH METERS (6 H, 0.75 CFU) TITRATION IN NON-AQUEOUS SOLVENTS: PRINCIPLES AND APPLICATIONS. (2H. 0.25CFU) INSTRUMENTAL METHODS: UV/VIS SPECTROPHOTOMETRY AND ITS APPLICATION IN THE QUANTITATIVE ANALYSIS OF DRUGS ACCORDING TO EUROPEAN PHARMACOPOEIA: PRINCIPLES. QUANTITATIVE ANALYSIS BY UV SPECTROPHOTOMETRY. INSTRUMENTAL METHODS: SPECTROPHOTOMETER DESCRIPTION AND USE (4 H, 0.50 CFU) HIGH PERFORMANCE LIQUID CHROMATOGRAPHY AND ITS APPLICATION IN THE QUANTITATIVE ANALYSIS OF DRUGS ACCORDING TO THE EUROPEAN PHARMACOPOEIA, CLASSIFICATION OF HPLC TECHNIQUES, STATIONARY PHASE (NP, RP, HILIC, SEC, IEX, CHIRAL) AND MOBILE PHASE, TRANSITION FROM HPLC TO UHPLC, INSTRUMENTATION (HPLC, UHPLC, HPLC-PREP) AND DETECTORS (UV, DAD, FLD, ELSD, RID). DEVELOPMENT, OPTIMIZATION AND VALIDATION OF AN ANALYTICAL METHOD USING HPLC OR UHPLC: QUANTIFICATION BY EXTERNAL STANDARD, QUANTITATION BY INTERNAL STANDARD (BOTH ANALOGUE AND ISOTOPICALLY LABELED), DETERMINATION OF THE LIMIT OF QUANTIFICATION AND DETECTION (LOD AND LOQ), DETERMINATION OF THE MATRIX EFFECT, RECOVERY, REPEATABILITY AND REPRODUCIBILITY. SAMPLE PREPARATION METHODS FOR HPLC/UHPLC ANALYSIS, SAMPLE PURIFICATION BY HPLC. DETERMINATION OF DRUGS BY OFFICIAL PHARMACOPOEIA: EXAMPLES, DETERMINATION OF IMPURITIES (12 H, 1.50 CFU) PRACTICE ACID BASE OXIDOMETRIC, COMPLEXOMETRIC TITRATIONS: (25 H, 2 CFU) CALCULATION EXERCISE (11 H, 0.5 CFU) INSTRUMENTAL ANALYSIS, SPECTROPHOTOMETRIC AND LIQUID CHROMATOGRAPHY: DOSAGE: (12 H, 1.5 CFU) |
| Teaching Methods | |
|---|---|
| THE TEACHING CONSISTS OF 48 HOURS OF LESSONS (6 CFU) AND 48 HOURS OF LABORATORY (4 CFU). FRONTAL LESSONS FOCUSED ON THE SOLUTION OF CALCULATION EXERCISES CONCERNING THE TOPICS COVERED IN LESSON WILL BE HELD TWO WEEKLY. TO ACCESS THE EXAM, THE STUDENT MUST TAKE AT LEAST 75% OF THE LABORATORY EXERCISES. |
| Verification of learning | |
|---|---|
| THE ACHIEVEMENT OF THE COURSE OBJECTIVES IS CERTIFIED BY PASSING AN EXAM WITH EVALUATION OUT OF THIRTY. THE EXAMINATION IS DIVIDED INTO THREE PROGRESSIVE AND CALENDARISED PHASES. FOR ACCESS TO THE NEXT PHASE, PASSING THE PREVIOUS TEST IS REQUIRED. STUDENTS ATTENDING AT LEAST 75% OF THE ATTENDANCE ARE OFFERED THE OPPORTUNITY TO TAKE 2 INTERCOMPENSE WRITTEN TESTS (TAKEN HALFWAY AND TOWARDS THE END OF THE PROGRAM) WHICH, IF BOTH WITH A POSITIVE RESULT (18/30), EXEMPT THEM FROM THE WRITTEN TEST EXAM IF ACHIEVED WITHIN THE FIRST TWO USEFUL APPEARANCES. THE FIRST TEST CONSISTS OF PASSING THE UNKNOWN LABORATORY TEST WHICH CONCERNS THE SOLUTION OF AN ANALYTICAL PROBLEM HAVING THE SUBJECT OF TOPICS COVERED IN THE PRACTICAL EXERCISES. THE WEIGHT OF THE NEXT TWO TESTS IS 50%. THE SECOND TEST CONSISTS IN THE SOLUTION OF FIVE CALCULATION EXERCISES, TO PASS THE TEST THE CORRECT SOLUTION OF AT LEAST THREE PROBLEMS IS REQUIRED. THE WRITTEN TEST HAS A DURATION OF TWO HOURS. A MARK OF AT LEAST 18/30 IS REQUIRED TO ACCESS THE THIRD TEST THE THIRD PHASE CONCERNS THE PASSING OF AN ORAL EXAMINATION WHICH PROVIDES FOR A DISCUSSION OF APPROXIMATELY 20 MIN. AIMED AT ASSESSING THE LEVEL OF KNOWLEDGE AND UNDERSTANDING ACHIEVED BY THE STUDENT ON THEORETICAL AND METHODOLOGICAL CONTENT INDICATED IN THE PROGRAM, AND VERIFYING COMMUNICATION SKILLS, PROPERTY OF LANGUAGE AND ORGANIZATION OF THE PRESENTATION ON TOPICS WITH THEORETICAL CONTENT. STUDENTS ATTENDING AT LEAST 75% OF THE ATTENDANCE ARE OFFERED THE OPPORTUNITY TO TAKE 2 INTERCOMPENSE WRITTEN TESTS (TAKEN HALFWAY AND TOWARDS THE END OF THE PROGRAM) WHICH, IF BOTH WITH A POSITIVE RESULT (18/30), EXEMPT THEM FROM THE WRITTEN TEST EXAM IF ACHIEVED WITHIN THE FIRST TWO USEFUL APPEARANCES. |
| Texts | |
|---|---|
| SLIDES PROVIDED BY THE TEACHER DURING THE COURSE SKOOG, WEST, HOLLER, CROUCH, FONDAMENTI DI CHIMICA ANALITICA, EDISES KOLTHOFF, SANDELL, MEEHAN, BRUCKENSTEIN, ANALISI CHIMICA QUANTITATIVA, PICCIN. WATSON, ANALISI FARMACEUTICA, EDISES KELLNER, MERMER, OTTO, WIDMER, CHIMICA ANALITICA, EDISES COZZI, PROTTI, RUARO, ANALISI CHIMICA STRUMENTALE, ZANICHELLI HARRIS D.C., CHIMICA ANALITICA QUANTITATIVA, ED. ZANICHELLI PORRETTA G.C., ANALISI DI PREPARAZIONI FARMACEUTICHE, ED. CISU NOVELLINO E., MARSEGLIA S., IACCARINO C., ANALISI CHIMICO FARMACEUTICA QUANTITATIVA |
| More Information | |
|---|---|
| LANGUAGE OF TEACHING: ITALIAN; LOCATION OF THE LECTURES: DEPARTMENT OF PHARMACY. FOR FURTHER INFORMATION CONTACT THE TEACHERS: ESOMMELLA@UNISA.IT TCIAGLIA@UNISA.IT MVIVIANO@UNISA.IT |
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