Ateneo - UPO

Qualitative chemical analysis of inorganic drugs: dry analysis, wet analysis for the identification of cations and anions. Qualitative chemical analysis of organic and organometallic drugs: elemental analysis, solubility assays, recognition reactions of the main functional groups. Determination of some chemical-physical constants. Separation, isolation and purification techniques. Filtration. Solvent extraction. Crystallization. Distillation. Thin layer chromatography. Qualitative analysis through Infrared Spectrophotometry and UV-Visible Spectrophotometry.

“Farmacopea Ufficiale europea”.
“Principi di Analisi Farmaceutica" Cavrini V. Andrisano V. Società Editrice Esculapio.
“Manuale di Analisi Qualitativa” Giuseppe Caliendo EdiSES Università.

The course aims to provide basic knowledge for the identification of compounds of pharmaceutical interest through the qualitative pharmaceutical analysis methodologies provided by the European Pharmacopoeia.
Fundamental notions will be provided on the chemical-physical properties of compounds of pharmaceutical interest of an inorganic, organic and metallorganic nature, as well as the principles and use of the techniques used in the separation and purification of a mixture of compounds.

Knowledge of general and inorganic chemistry, analytical chemistry, physical chemistry and organic chemistry.

Lectures in the classroom with slide projection, some topics will be explored in depth with the projection of films. The teaching material used during the lessons will be available on the DIR platform.
Practical laboratory exercises, mandatory attendance.

Students with physical disabilities, Learning Disabilities or Special Education Needs can request specific services and tools via the Staff Sviluppo e Coordinamento Carriere e Servizi alle Studentesse e agli Studenti, consulting the University webpage: https://www.uniupo.it/en/services/services-students-physical-or-learning-disabilities
Students with disabilities, learning disabilities or special education needs, once they have contacted the University Staff, can refer to the tutor in charge of the course to define the examination modalities, concerning academic aspects.

There is a MANDATORY ongoing written test prior to entry to the laboratory. The written test will take place as soon as the lectures are finished and will cover all the topics covered in the course. In the written test, 30 questions will be asked: both multiple choice and open-ended.
The student who obtains a grade equal to or higher than 18/30 in the written test will attend the laboratory and obtain an evaluation of the analyzes carried out. The final mark will take into account both the mark obtained in the written test and the result of the analyzes carried out during the laboratory exercises. The vote will be recorded at the first available minutes.
Students who obtain a grade lower than 18/30 in the written test will be admitted to attend the laboratory, but will have to take a second written test at the end of the laboratory. If the result of the second written test is still insufficient, students will have to register for the exams and take both a written test and an oral test.

LABORATORY GLASSWARE: use, maintenance and typical assembly of standard apparatus.

STIRRING, HEATING, COOLING TECHNIQUES.

QUALITATIVE CHEMICAL ANALYSIS: sampling and homogenization of the sample, preliminary analyses: appearance, color, odor, determination of the organic, inorganic, metal-organic nature by calcination test on earthenware; dry analysis (flame test and heating tests in a small tube).

QUALITATIVE CHEMICAL ANALYSIS OF INORGANIC SUBSTANCES:
- dissolution, pH measurement, possible fusion
- wet analysis: identification of cations and anions present in samples of inorganic drugs through characteristic chemical reactions described in the Pharmacopoeia, with particular reference to the following cations (Ammonium, Aluminium, Silver, Bismuth, Calcium, Lithium, Magnesium, Potassium, Sodium, Zinc) and anions (Carbonates, Bicarbonates, Chlorides, Phosphates, Iodides, Nitrates, Sulphates, Borates, Fluorides, Thiosulfates).

QUALITATIVE CHEMICAL ANALYSIS OF ORGANIC AND METALLORGANIC SUBSTANCES:
- elemental analysis: Lassaigne assay searches for nitrogen, sulphur, halogens and phosphorus
- dry analysis (flame test for organometallic compounds)
- solubility tests in water, organic solvents, diluted bases, diluted acids, conc sulfuric acid.
- recognition reactions of the main functional groups: alkenes, alkynes, aromatic hydrocarbons, alkyl halides, alcohols, phenols, ethers, aldehydes, ketones, carboxylic acids, acyl halides, anhydrides, esters, amides, nitriles, amines and ammonium salts, nitro -compounds, sulphonamides, amino acids, carbohydrates
- use of the Pharmacopoeia: examples of recognition of some organic and organometallic drugs: acetylsalicylic acid, salicylic acid, bismuth salicylate, chlorobutanol, hexylresorcin, glucose, fructose, sucrose, benzocaine, procaine hydrochloride, sulfathiazole.

DETERMINATION OF CHEMICAL-PHYSICAL CONSTANTS:
- Melting point.
- Specific rotational power.

SEPARATION, ISOLATION AND PURIFICATION TECHNIQUES:
- FILTRATION: by gravity and vacuum, filtration auxiliaries, microfiltration, centrifugation, decantation, drying methods.
- SOLVENT EXTRACTION: principle and choice of solvent, discontinuous liquid-liquid extraction method with separating funnel, phase washing, anhydrification and concentration.
Use of acidic aqueous solutions and basic aqueous solutions. Continuous liquid-liquid extraction method: continuous extractors for solvents denser than water; continuous extractors for solvents less dense than water. Continuous solid-liquid extraction method: Soxhlet.
- CRYSTALLIZATION: principle and procedures.
- DISTILLATION: simple and fractional room pressure distillation; simple and fractional vacuum distillation; steam distillation.
- THIN LAYER CHROMATOGRAPHY: methodology, applications, RF calculation, detection systems, two-dimensional TLC, preparative TLC.

INFRARED SPECTROPHOTOMETRY: instrumentation and applications in qualitative pharmaceutical analysis, interpretation of IR spectra.

UV-Visible SPECTROPHOTOMETRY: instrumentation and applications in qualitative pharmaceutical analysis.

LABORATORY EXERCISES: Drug calcination assays, Lassaigne assay and elemental analysis. Identification of unknown inorganic drugs and confirmation of the identity of organic and organometallic drugs according to the European Pharmacopoeia. Purification of a drug present in a mixture using the solvent extraction technique. Identification of drugs through IR Spectrophotometry and UV-Visible Spectrophotometry according to Pharmacopoeia.

At the end of the course, the student will acquire the basic knowledge to carry out the identification of compounds of pharmaceutical interest of an inorganic, organic and metal-organic nature registered in the European Pharmacopoeia. In particular, the student will be able to perform solubility tests, specific chemical tests, will be able to determine some chemical-physical constants and apply knowledge of IR and UV/Visible spectrophotometry to identify an active pharmaceutical ingredient. Furthermore, students will be able to perform the main separation, isolation and purification techniques of compounds of pharmaceutical interest.