PHARMACEUTICAL ANALYSIS I

TANIA CIAGLIA PHARMACEUTICAL ANALYSIS I

0760200009
DIPARTIMENTO DI FARMACIA
EQF7
PHARMACEUTICAL CHEMISTRY AND TECHNOLOGY
2023/2024

OBBLIGATORIO
YEAR OF COURSE 2
YEAR OF DIDACTIC SYSTEM 2020
AUTUMN SEMESTER
CFUHOURSACTIVITY
648LESSONS
448LAB


Objectives
THE COURSE HAS THE OBJECTIVE OF
PROVIDE THE STUDENT WITH THE THEORETICAL, PRACTICAL AND METHODOLOGICAL CONCEPTS TO CARRY OUT THE QUANTITATIVE ANALYSIS OF MOLECULES OF PHARMACEUTICAL, NUTRACEUTICAL AND COSMECEUTICAL INTEREST THROUGH CLASSICAL AND ADVANCED/INSTRUMENTAL ANALYSIS APPROACHES DESCRIBED IN THE MAIN PHARMACOPOEIES.
KNOWLEDGE AND UNDERSTANDING
AT THE END OF THE COURSE THE STUDENT WILL KNOW THE RELATED THEORETICAL PRINCIPLES: - THE METHODS OF PURIFICATION AND QUANTITATIVE ANALYSIS OF BEES WITH PARTICULAR CONCERNING THOSE LISTED IN THE PHARMACOPOEIES; - CALCULATION APPROACHES FOR THE SOLUTION OF 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 THROUGH SEPARATION TECHNIQUES, PURIFICATION OF MOLECULES OF PHARMACEUTICAL INTEREST.
ABILITY TO APPLY KNOWLEDGE AND UNDERSTANDING
AT THE END OF THE COURSE THE STUDENT WILL BE ABLE TO:
- DESCRIBE THE THEORETICAL AND PRACTICAL ASPECTS OF THE CLASSICAL AND ADVANCED CHEMICAL-PHARMACEUTICAL ANALYSIS METHODS; - QUANTITATIVELY ANALYZE USING CLASSICAL, INSTRUMENTAL (CHROMATGRAPHIC/SPECTROSCOPIC) TECHNIQUES OF MOLECULES OF PHARMACEUTICAL INTEREST; - PROCESS THE QUANTITATIVE DATA OBTAINED IN A STATISTICALLY CRITICAL MANNER AND ASSESS THEIR VALIDITY; - SOLVING CALCULATION EXERCISES RELATING TO THE DOSAGE OF MIXTURES OF PHARMACEUTICAL AND/OR NUTRACEUTICAL/COSMECEUTICAL INTEREST.
AUTONOMY OF JUDGMENT
- EVALUATE THE PROCEDURES USED WITH A CRITICAL SENSE, THROUGH THE USE OF CALCULATIONS, STATISTICAL APPROACHES AND VALIDATION OF THE RESULTS; - DESIGN PROTOCOLS FOR THE QUANTITATIVE DETERMINATION OF APIS AND IMPURITIES DESCRIBED IN THE MAIN PHARMACOPOEIES; - SELECT THE MOST APPROPRIATE METHODS FOR THE PURIFICATION, SEPARATION AND QUANTITATIVE DETERMINATION OF MOLECULES OF PHARMACEUTICAL INTEREST
COMMUNICATION SKILL
- COMMUNICATE AND PRESENT BY MEANS OF REPORTS ALSO IN DIGITAL FORMAT, AND IN A MULTIDISCIPLINARY FIELD, THE RESULTS OF THE MOST SUITABLE PROTOCOLS FOR THE RESOLUTION OF PROBLEMS RELATED TO THE QUANTITATIVE DETERMINATION OF MOLECULES OF PHARMACEUTICAL, NUTRACEUTICAL AND COSMECEUTICAL INTEREST LEARNING SKILLS - USE THE STR ACQUIRED MENTS FOR THE CRITICAL EVALUATION OF TEXTS SUCH AS PHARMACOPOEIA MONOGRAPHS, OR CERTIFIED ANALYSIS METHODS OR DESCRIBED IN THE LITERATURE FOR THE QUANTITATIVE DETERMINATION OF APIS AND IMPURITIES AND THE SELECTION, IN THE FIELD 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.
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
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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