DRUG ANALYSIS I

VERONICA DI SARNO DRUG ANALYSIS I

0760300008
DIPARTIMENTO DI FARMACIA
EQF7
PHARMACY
2023/2024

OBBLIGATORIO
YEAR OF COURSE 2
YEAR OF DIDACTIC SYSTEM 2023
SPRING SEMESTER
CFUHOURSACTIVITY
648LESSONS
672LAB


Objectives
THIS COURSE IS AIMED AT OBTAINING KNOWLEDGE AND UNDERSTANDING OF:
-THEORETICAL PRINCIPLES AND PRACTICAL ASPECTS FOR THE CONTROL OF THE PURITY
OF PHARMACEUTICAL SUBSTANCES AND FOR THE QUANTITATIVE DETERMINATION
OF BIOACTIVE COMPOUNDS CONTAINED IN THE MOST MEDICINAL SPECIALTIES, IN
ACCORDING TO OFFICIAL ITALIAN AND EUROPEAN PHARMACOPOEIA.
-MAIN ANALYTICAL METHODOLOGIES AND INSTRUMENTAL TECHNIQUES USED FOR
THE QUANTITATIVE ANALYSIS OF DRUGS
THE STUDENT, BASED ON THE ACQUIRED SKILLS, WILL BE ABLE TO:
-CARRY OUT QUANTITATIVE ANALYSIS OF PHARMACEUTICAL SUBSTANCES IN
ACCORDING TO THE MONOGRAPHS OF OFFICIAL PHARMACOPOEIA
- DEVELOP AND VALIDATE QUANTITATIVE ANALYTICAL PLATFORMS ACCORDING TO
THE CHEMICAL STRUCTURE OF THE ANALYTES, THE PROPERTIES OF THE
INVESTIGATED MATRICES AND THE REQUIRED SENSITIVITY
- CRITICAL EVALUATION OF THE RESULTS
Prerequisites
THE STUDENT MUST HAVE PASSED THE GENERAL AND INORGANIC CHEMISTRY AND ANALYTICAL CHEMISTRY EXAM AND INTRODUCTION TO DRUG ANALYSIS.
ALSO, THE ACQUISITION OF THE OBJECTIVES OF THE ORGANIC CHEMISTRY COURSE IS STRONGLY RECOMMENDED.
Contents
LECTURES (48 HOURS- 6 ECTS )

SAFETY IN LABORATORIES. REGULATIONS. THE ITALIAN OFFICIAL PHARMACOPOEIA (F.U.). THE EUROPEAN PHARMACOPOEIA (E.P.). GLASSWARE AND ITS USE. ELECTRONIC SCALES, CONCENTRATION UNITS. (4 HOURS- 0.5 ECTS).
SCALE OF WORK. NORMALITY, EQUIVALENT, CALCULATIONS IN VOLUMETRIC ANALYSIS (2 HOURS- 0.25 ECTS).
ANALYSIS OF THE PH OF STRONG AND WEAK ACIDS AND BASES. CALCULATION OF PH OF POLYPROTIC ACIDS AND THEIR SALTS. TITRATION CURVES OF ACIDS AND BASES. THEORY OF INDICATORS. MAIN ACID-BASE INDICATORS AND THEIR USE. PRIMARY STANDARDS, THEIR CHARACTERISTICS AND THEIR USE. STANDARD SOLUTIONS OF ACIDS AND BASES USED IN VOLUMETRIC ANALYSIS. EXAMPLES OF TITRATIONS ACCORDING TO E.P. (10 HOURS- 1.25 ECTS)
SOLUBILITY. SOLUBILITY PRODUCT. PRECIPITATION AND REDISSOLUTION OF THE PRECIPITATES. COLLOIDAL PRECIPITATES (2 HOURS- 0.25 ECTS).
TITRATION CURVES OF PRECIPITATION. DETERMINATION OF HALIDES ACCORDING TO MOHR, VOLHARD, FAJANS AND LIEBIG-DENIGES. PREPARATION OF STANDARD SOLUTIONS USED IN PRECIPITATION ANALYSIS. EXAMPLES OF DETERMINATIONS OF PRECIPITATION (4 HOURS- 0.5 ECTS).
COMPLEXOMETRIC TITRATION. METALLOCROMIC INDICATORS. COMPLEX-FORMATION AND INSTABILITY CONSTANTS. EXAMPLES OF COMPLEXOMETRIC TITRATIONS ACCORDING TO E.P. (4 HOURS- 0.5 ECTS)
DEFINITION AND USE OF THE STANDARD REDUCTION POTENTIAL. REDOX INDICATORS AND SPECIFIC INDICATORS (2 HOURS- 0.25 ECTS). PERMANGANOMETRY. IODIMETRY. IODOMETRY. CERIMETRY. BROMATOMETRY (10 HOURS- 1.25 ECTS).
COMPLEXATION
TITRATIONS IN NONAQUEOUS SOLVENTS: THEORY AND APPLICATIONS (2 HOURS- 0.25 ECTS).
UV/VIS SPECTROPHOTOMETRY, THEORETICAL ASPECTS AND PRACTICAL APPLICATIONS. LAMBERT-BEER'S LAW. (2 HOURS- 0.25 ECTS)
QUANTITATIVE ANALYSIS USING HPLC HIGH PERFORMANCE CHROMATOGRAPHY (6 HOURS- 0.75 ECTS)


PRACTICALS (72 HOURS-6 ECTS)

STANDARDIZATION OF AN APPROXIMATE NAOH SOLUTION AND QUANTITATIVE DETERMINATION OF A MONOPROTIC ACID AND OF A POLYPROTIC ACID (6 HOURS - 0.5 ECTS)
QUANTITATIVE DETERMINATION OF THE CONSTITUENTS OF AN UNKNOWN ALKALINE MIXTURE (3 HOURS - 0.25 ECTS)
CONSTRUCTION OF TWO TITRATION CURVES USING HYDROCHLORIC ACID AS TITRATING AGENT AND SODIUM HYDROXIDE AND SODIUM CARBONATE AS ANALYTE (3 HOURS - 0.25 ECTS)
DETERMINATION OF THE PROTEIN CONTENT ACCORDING TO THE KJELDAHL METHOD (3 HOURS - 0.25 ECTS)
QUANTITATIVE DETERMINATION OF AN UNKNOWN CONCENTRATION SOLUTION OF NACL BY APPLYING THE MOHR METHOD, THE FAJANS METHOD AND THE VOLHARD METHOD (6 HOURS - 0.5 ECTS)
DETERMINATION OF TOTAL WATER’S HARDNESS, AND CALCIUM AND MAGNESIUM CONTENT OF A SAMPLE OF WATER USING A SOLUTION OF EDTA AGENT (3 HOURS - 0.25 ECTS)
DETERMINATION OF OXYGEN VOLUMES OF HYDROGEN PEROXIDE SOLUTION USING A SOLUTION OF POTASSIUM PERMANGANATE (3 HOURS - 0.25 ECTS)
QUANTITATIVE DETERMINATION OF THE ASCORBIC ACID USING A SOLUTION OF IODINE (3 HOURS - 0.25 ECTS)
QUANTITATIVE DETERMINATION OF ACTIVE INGREDIENTS OF PHARMACEUTICAL INTEREST THROUGH SPECTROPHOTOMETRIC ANALYSIS (UV/VIS) (6 HOURS - 0.5 ECTS)
QUANTITATIVE DETERMINATION OF ACTIVE INGREDIENTS OF PHARMACEUTICAL INTEREST THROUGH CHROMATOGRAPHIC ANALYSIS (UV/VIS) (12 HOURS - 1 ECTS)
GUIDED SOLUTION AND RELATED CRITICAL DISCUSSION OF EXERCISES CONCERNING THE TOPICS COVERED (24 HOURS – 2.0 ECTS)
Teaching Methods
THE COURSE CONSISTS OF 120 HOURS OF LESSONS (12 ECTS) DIVIDED INTO 48 HOURS OF THEORETICAL LESSONS (6 ECTS) AND 72 HOURS OF LABORATORY (6 ECTS) OF WHICH 48 HOURS OF GUIDED EXERCISES IN THE LAB, IN A SINGLE PLACE, FOR THE QUANTITATIVE ANALYSIS OF ACTIVE INGREDIENTS OF PHARMACEUTICAL INTEREST, AND 24 HOURS OF CALCULATION EXERCISES CONCERNING THE TOPICS COVERED.
THE LECTURES ARE DELIVERED IN THE CLASSROOM WITH THE AID OF PROJECTIONS AND DEAL WITH ALL THE TOPICS OF THE COURSE PROGRAMME.
BEFORE EACH LABORATORY EXERCISE, STUDENTS WILL BE DULY INSTRUCTED AND PROVIDED WITH MATERIAL RELATING TO THE EXERCISE ITSELF.
WEEKLY LESSONS FOCUSED ON THE SOLUTION OF CALCULATION EXERCISES RELATING TO THE TOPICS COVERED WILL BE HELD.
THE ATTENDANCE OF LESSONS BOTH IN THE CLASSROOM AND IN THE LABORATORY IS MANDATORY.
THE FREQUENCY OF AT LEAST 80% OF LABORATORY LESSONS AND AT LEAST 70% OF FRONTAL LESSONS ARE REQUIRED FOR THE ACCESS TO THE EXAM.
Verification of learning
THE ACHIEVEMENT OF THE COURSE OBJECTIVES IS CERTIFIED BY THREE FOLLOWING TESTS. THE FIRST ONE CONSISTS IN A LABORATORY TEST CONCERNING THE TITRATION OF A SPECIFIC CHEMICAL COMPOUND.
THE SECOND ONE IS A WRITING TEST COMPOSED BY 5 DIFFERENT ANALYTICAL PROBLEMS AND THE CORRECT RESOLUTION OF AT LEAST THREE PROBLEMS IS REQUIRED. THE LAST TEST IS A 20 MINUTES ORAL TEST AIMED TO ENSURE THE STUDENT’S KNOWLEDGE ABOUT THEORETICAL AND METHODOLOGICAL TOPICS. THE ORAL TEST IS ALSO AIMED TO VERIFY THE COMMUNICATION AND LANGUAGE SKILLS.
THE FINAL MARK WILL TAKE IN ACCOUNT THE RESULTS OF THE PRATICAL, WRITTEN AND THE ORAL TESTS.
Texts
-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
- BIOANALYSIS OF PHARMACEUTICALS: SAMPLE PREPARATION, SEPARATION TECHNIQUES AND MASS SPECTROMETRY, FIRST EDITION. STEEN HONORÉ HANSEN AND STIG PEDERSEN-BJERGAARD. © 2015 JOHN WILEY & SONS, LTD. PUBLISHED 2015 BY JOHN WILEY & SONS, LTD.
-OTHER EDUCATIONAL MATERIAL: THE EDUCATIONAL MATERIAL IS PROVIDED DURING LESSON AND AVAILABLE ON THE TEACHER'S WEBSITE.
More Information
THE COURSE WILL BE IN ITALIAN. FOR MORE INFO CONTACT VDISARNO@UNISA.IT
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