DRUG ANALYSIS II

MARIA CARMINA SCALA DRUG ANALYSIS II

0760300021
DIPARTIMENTO DI FARMACIA
EQF7
PHARMACY
2023/2024

OBBLIGATORIO
YEAR OF COURSE 4
YEAR OF DIDACTIC SYSTEM 2023
SPRING SEMESTER
CFUHOURSACTIVITY
648LESSONS
448LAB


Objectives
THIS TEACHING IS AIMED AT PROVIDING THE STUDENT WITH THE SKILLS NECESSARY FOR THE SELECTION OF THE CORRECT ANALYTICAL WORKFLOW FOR THE IDENTIFICATION OF COMPOUNDS OF PHARMACEUTICAL INTEREST THROUGH INSTRUMENTAL ANALYTICAL TECHNIQUES AND SPECIFIC CHEMICAL ASSAYS. THE STUDENT WILL ACQUIRE THE ABILITY TO UNDERSTAND AND APPLY THE METHODS REPORTED IN THE LATEST EDITION OF THE EUROPEAN PHARMACOPOEIA. THE SET OF THEORETICAL AND PRACTICAL KNOWLEDGE ACQUIRED ALLOWS STUDENTS TO DESIGN AND IMPLEMENT, INDEPENDENTLY, ANALYTICAL-QUALITATIVE PROCEDURES TO BE USED IN THE PHARMACEUTICAL FIELD, ALSO ALLOWING THE COMPLETION OF THE SPECIFIC FEATURES BELONGING TO THE CULTURAL IDENTITY OF THE GRADUATE IN PHARMACY.

AT THE END OF THE TEACHING COURSE, THROUGH THE USE OF THE PROPOSED TEACHING MATERIAL AND TAKING ADVANTAGE OF THE LECTURES GIVEN AND THE RELATED LABORATORY EXERCISES, THE STUDENTS WILL POSSESS THEORETICAL AND PRACTICAL KNOWLEDGE CONCERNING:

- ANALYTICAL METHODS FOR DETERMINATION OF THE CHEMICAL-PHYSICAL PROPERTIES CHARACTERIZING SUBSTANCES, IN PARTICULAR THE CHEMICAL SUBSTANCES OF PHARMACEUTICAL INTEREST (BOILING POINT, MELTING POINT, DENSITY, REFRACTIVE INDEX, SPECIFIC ROTATIONAL POWER)
- STRUCTURAL AND CHEMICAL CHARACTERIZATION TECHNIQUES OF ORGANIC COMPOUNDS THROUGH THE KNOWLEDGE OF SPECTROSCOPIC AND CHEMICAL RECOGNITION TECHNIQUES.
- SPECIFIC PROCEDURES RELATED TO THE RECOGNITION OF COMPOUNDS DESCRIBED IN THE EUROPEAN PHARMACOPOEIA
- METHODS FOR THE SEPARATION, PURIFICATION AND IDENTIFICATION OF ORGANIC COMPOUNDS STARTING FROM COMPLEX MIXTURES (CHROMATOGRAPHY, EXTRACTION, DISTILLATION, SUBLIMATION, CRYSTALLIZATION)

THROUGH INDIVIDUAL LABORATORY CLASSES, THE STUDENT APPLIES THE THEORETICAL METHODS TO THE SEPARATION, PURIFICATION AND IDENTIFICATION OF ORGANIC COMPOUNDS WITH A SPECIFIC INTEREST IN PHARMACEUTICAL INGREDIENTS. STUDENTS ARE EXPECTED TO DEMONSTRATE THAT THEY ARE CAPABLE OF APPLYING THEIR KNOWLEDGE AND UNDERSTANDING IN A PRACTICAL CONTEXT BY PROVIDING TECHNICAL-PROFESSIONAL SOLUTIONS TO ANALYTICAL-QUALITATIVE PROBLEMS FOR THE SEPARATION AND RECOGNITION OF AN UNKNOWN SUBSTANCE, ALSO IN ACCORDANCE WITH THE METHODS DESCRIBED IN THE EUROPEAN PHARMACOPOEIA.
Prerequisites
IN ORDER TO HAVE ACCESS TO THE FINAL EXAM, THE STUDENT MUST HAVE PASSED ALL THE EXAMS OF THE SECOND YEAR OF THE RPOGRAMME
Contents
THE COURSE IS DIVIDED INTO A THEORETICAL PART (48 HOURS, 6 CREDITS) AND A PRACTICAL PART (48 HOURS, 4 CREDITS).
THE THEORETICAL COURSE INCLUDES THE FOLLOWING TOPICS:
- PRESENTATION OF THE COURSE, ORGANOLEPTIC ANALYSIS AND PHARMACOPOEIA (2 HOURS - 0.25 CFU)
-ANALYSIS OF PURE SUBSTANCES: CHEMICAL-PHYSICAL PROPERTIES: COMBUSTION BEHAVIOR, OPTICAL ACTIVITY, REFRACTIVE INDEX, DENSITY, MELTING POINT AND BOILING POINT. (4 HOURS - 0.50 CREDITS)
-PHYSICAL CONSTANTS AND SOLUBILITY: ANALYSIS AND RELATIONSHIP WITH THE STRUCTURE (4 HOURS, 0.50 CFU).
- QUALITATIVE ORGANIC ELEMENTAL ANALYSIS: LASSAIGNE TEST: SEARCH FOR CARBON AND HYDROGEN, NITROGEN, SULFUR AND HALOGENS; COMBUSTION ASSAYS, BEILSTEIN ESSAY (2 HOURS - 0.25 CFU)
- GENERAL ASSAYS: UNSATURATION ASSAY, AROMATIC RING ASSAY. CHEMICAL ASSAYS FOR THE IDENTIFICATION OF THE MAIN FUNCTIONAL GROUPS: CARBOXYLIC ACIDS AND DERIVATIVES; ALDEHYDES AND KETONES; ACETALS AND KETALS: CARBOHYDRATES; ALCOHOLS AND PHENOLS; AMINES; AMINO ACIDS; ALKALOIDS. ANALYTICAL PROFILE OF SOME DRUG CLASSES: ALKALOIDS, BENZODIAZEPINES, BARBITURATES, STEROIDS. (16 HOURS - 2.00 CREDITS)
- MAIN PURIFICATION TECHNIQUES: EXTRACTION, CRYSTALLIZATION AND DISTILLATION. (4 HOURS - 0.50 CREDITS)
-THEORETICAL ASPECTS OF CHROMATOGRAPHY (CLASSICAL CHROMATOGRAPHY, FLASH, TLC, GC, HPLC, UPLC). (4 HOURS –0.50 CREDITS)
- SPECTROSCOPIC METHODS: (UV, IR, NMR). (8 HOURS – 1.00 CREDITS)
-MAIN SEPARATION TECHNIQUES (STAUDINGER METHOD). (4 HOURS - 0.50 CREDITS)

THE PRACTICAL PART COVERS THE FOLLOWING TOPICS:
-SAFETY IN THE LABORATORY. ACQUISITION OF TERMINOLOGY AND INTRODUCTION TO LABORATORY PRACTICE. RECOGNITION OF GLASSWARE AND ITS CORRECT USE TO ANALYZE AN ORGANIC DRUG. (4 HOURS - 0.33 CREDITS)
-CHEMICAL-PHYSICAL CHARACTERISTICS: ORGANOLEPTIC EXAMINATION, DETERMINATION OF THE MELTING POINT, DETERMINATION OF DENSITY (5 HOURS, 0.42 CFU).
-DETERMINATION OF THE SOLUBILITY PROFILE OF SUBSTANCES OF PHARMACEUTICAL INTEREST BY VISUAL INSPECTION (4 HOURS, 0.33 CFU).
-IDENTIFICATION REACTIONS FOR CARBOXYLIC ACIDS, ALCOHOLS AND PHENOLS (5 HOURS, 0.42 CFU).
-IDENTIFICATION REACTIONS FOR ALDEHYDES, KETONES AND SUGARS (5 HOURS, 0.42 CFU).
- IDENTIFICATION REACTIONS FOR AMINES, AMINO ACIDS AND SOME ALKALOIDS (5 HOURS, 0.42 CFU)
- SEPARATION AND PURIFICATION METHODS: SEPARATION BY LIQUID-LIQUID EXTRACTION OF MIXED ORGANIC COMPOUNDS AND ANALYSIS BY THIN LAYER CHROMATOGRAPHY (5 HOURS, 0.42 CFU).
- QUALITATIVE ANALYSIS OF ORGANIC COMPOUNDS USING HPLC (5 HOURS, 0.42 CFU).
-SPECTROSCOPIC ANALYSIS OF ORGANIC COMPOUNDS FROM FU: (4 HOURS, 0.42 CFU).
- LABORATORY EXAM: RECOGNITION OF 2/4 UNKNOWN SAMPLES CONTAINING ORGANINC SUBSTANCES OF PHARMACEUTICAL INTEREST (5 HOURS, 0.42 CFU).
Teaching Methods
THE COURSE IS DIVIDED INTO A THEORETICAL AND A PRACTICAL PART.
THE THEORETICAL PART INCLUDES FRONTAL LESSONS FOR A TOTAL OF 48 HOURS (6 CREDITS), WHICH TAKE PLACE IN THE CLASSROOMS USING PROJECTION DEVICES.
THE PRACTICAL PART INCLUDES INDIVIDUAL PRACTICE IN THE TEACHING LABORATORY REGARDING THE SAME TOPICS ALREADY COVERED IN THE THEORETICAL LESSONS FOR A TOTAL OF 48 HOURS (4 CFU)
BEFORE EACH LABORATORY, STUDENTS WILL BE DULY INSTRUCTED AND PROVIDED WITH MATERIAL REGARDING THE ACTIVITY TO BE EXECUTED.
IN ORDER TO BE ABLE TO ATTEND TO THE FINAL EXAM, THE STUDENT MUST HAVE ATTENDED AT LEAST 80% OF THE PLANNED LABORATORY CLASSES.
Verification of learning
THE ACHIEVEMENT OF THE COURSE OBJECTIVES IS CERTIFIED BY PASSING A FINAL EXAM. THE EXAM IS DIVIDED INTO THREE PROGRESSIVE AND SCHEDULED PHASES: A LABORATORY TEST, A WRITTEN TEST AND AN ORAL TEST WHICH TAKE PLACE ON DIFFERENT DAYS. A POSITIVE EVALUATION IN EACH PHASE IS A PREREQUISITE FOR THE ACCESS TO THE NEXT PHASE.

A) LABORATORY TEST: REQUIRES IDENTIFICATION OF 2/4 UNKNOWN SAMPLES.
THE EVALUATION OF THE LABORATORY FINAL EXAM (PASSED / FAILED ) WILL TAKE INTO CONSIDERATION BOTH THE STUDENT'S SKILLS IN CORRECTLY CARRYING OUT THE ANALYSIS AND THE ABILITY TO SCRUPULOUSLY FOLLOW THE SAFETY REGULATIONS.
B) WRITTEN TEST: SIX OPEN-ENDED QUESTIONS, TREATING GENERAL THEORETICAL ASPECTS.
THE TEST HAS A DURATION OF NO LESS THAN 90 MINUTES AND IS AIMED AT VERIFYING THE ACQUISITION OF THE MINIMUM LEARNING OBJECTIVES.
C) ORAL EXAM: THE ORAL EXAM, LASTING ABOUT 30 MINUTES, CONSISTS OF AN INTERVIEW AIMED AT ASCERTAINING THE LEVEL OF UNDERSTANDING ACHIEVED BY THE STUDENT ON THE CONTENTS INDICATED IN THE PROGRAM AND THE STUDENT'S ABILITY TO APPLY THE ACQUIRED KNOWLEDGE. THE ORAL TEST WILL ALSO ALLOW TO VERIFY THE STUDENT'S COMMUNICATION SKILLS WITH PARTICULAR ATTENTION TO THE PROPERTY OF LANGUAGE AND THE AUTONOMOUS ORGANIZATION OF THE DISSERTATION.
THE FINAL GRADE OF THE EXAM WILL BE THE COMBINED RESULT OF THE WRITTEN AND ORAL EXAMS.
DURING THE COURSE, THE STUDENT ALSO HAS THE OPPORTUNITY TO CARRY OUT TWO MIDTERM TESTS (PIT). IN ORDER TO ACCESS TO THE MIDTERM TESTS, THE STUDENT MUST HAVE ATTENDED AT LEAST 70% OF THE CLASSES.
A SCORE BETWEEN 18 AND 30 WILL BE ASSIGNED FOR EACH SINGLE TEST PASSED. THE FINAL RESULT OF THE MIDTERM TESTS WILL BE THE MATHEMATICAL AVERAGE OF THE SCORES GIVEN. THE MIDTERM TESTS WILL BE SCHEDULED YEARLY WITH THE STUDENTS.
PASSING THE MIDTERM EXAMS IS CONSIDERED A SUBSTITUTE FOR THE WRITTEN EXAM.
Texts
THE SLIDES OF THE LESSONS, PROVIDED BY THE PROFESSOR, CAN BE CONSIDERED AS DIDACTIC MATERIAL.
FURTHER INFORMATION CAN BE OBTAINED USING THE FOLLOWING TEXTBOOKS:
SAVELLI, O. BRUNO; ANALISI CHIMICO FARMACEUTICA, PICCIN
SHRIRER ET AL.;THE SYSTEMATIC IDENTIFICATION OF ORGANIC COMPOUNDS, WILEY
V. CAVRINI, V. ANDRISANO; ANALISI FARMACEUTICA – METODI DI RICONOSCIMENTO E DI SEPARAZIONE, ESCULAPIO
ARANEO, LIVERANI; ANALISI CHIMICA QUALITATIVA, AMBROSIANA
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