Ateneo - UPO

Qualitative chemical analysis of inorganic drugs: identification of cations and anions
Qualitative chemical analysis of organic and metalorganic drugs: elemental analysis, determination of solubility, chemical tests for the characterization of functional groups.
Determination of chemical-physical constants.
Thin layer chromatography.
Extraction and purification with solvent:
Infrared spectrometry.
UV/Visible spectrometry.

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

The aim of this course is to provide the basic knowledge for the identification process of known and unknown compounds of pharmaceutical interest according to Farmacopea Ufficiale Italiana and “European Pharmacopoeia”.

Medicinal Analysis I (before 30 September)

Frontal lectures in the first semester and practical lessons in the laboratory in the second semester, compulsory attendance.

A compulsory written test is required preceding the entrance to the laboratory. The written test will take place in February and will cover all the topics discussed during the theoretical lessons.
In the written test, 30 questions will be asked: many with multiple choice and some with open response.
The student who has received an evaluation in the written test ≥ 18/30 will attend the laboratory and will receive a lab score. The final evaluation will take into account both the marks obtained in the written test and the results of the analyzes carried out during laboratory practice. The final mark will be recorded at the first available call.
The student, who has received an evaluation in the written test ˂18/30, will have the opportunity to hold a second written test in the same month. If the outcome of the second test is still insufficient, the student will have a thid written test available, which represents the last chance to be admitted to attend the laboratory scheduled in the second semester.

QUALITATIVE CHEMICAL ANALYSIS: sampling and homogenization of compounds; preliminary examination: physical state, color, odor; determination of inorganic, organic and metalorganic nature of the compounds by ignition test; dry test (flame test )
Qualitative chemical analysis of inorganic compounds:
- solubility, determination of pH,
- wet test: identification of cations (NH4+, Al+++, Ag+, Bi+++, Ca++, Li+, Mg++, K+, Na+, Zn++) and anions (CO3- -, HCO3 -, Cl -, PO4- - -, I -, NO3 -, SO4- - , BO3- - -, F -, S2O3- -) contained in inorganic drugs, adopting methods of identification described in the European Pharmacopoeia.
Qualitative chemical analysis of organic and metalorganic compounds:
- elemental analysis: Lassaigne test (fusion with sodium) for the determination of the presence of nitrogen, sulfur, chlorine, bromine, iodine, fluorine and phosphorus.
- dry test (flame test for metalorganic compounds)
- Theory of solubility, determination of solubility in water, organic solvent (ether), 5% hydrochloric acid solution, 5% sodium hydroxide solution, 5% sodium bicarbonate solution and cold concentrated sulfuric acid.
- Chemical tests for the characterization of functional groups: alkenes, alkynes, aromatic hydrocarbons, halides, alcohols, phenols, ethers, aldehydes, ketones, carboxylic acids, acyl halides, acid anhydrides, esters, amides, nitriles, amines, nitro-compounds, sulfonamides, amino acids, carbohydrates
-use of the European Pharmacopoeia
- determination of chemical-physical constants: melting point, (mixed melting point method, corrected melting point); polarimetry: specific rotation.
THIN LAYER CHROMATOGRAPHY (TLC): technique, application, determination of Rf value and Rstd value, detection methods, bidimensional TLC, preparative TLC.
INFRARED SPECTROMETRY: theory, schematic diagram of spectrometers, application, study of the IR spectra of several organic compounds.
UV/VISIBLE SPECTROMETRY: theory, schematic diagram of spectrometers, applications.
EXTRACTION AND PURIFICATION WITH SOLVENT: purpose, solvent choice, extraction technique with separation funnel, methods of extraction: solvent/water, solvent/acid aqueous solution, solvent/basic aqueous solution.
PRACTICAL LESSONS: Ignition test of compounds, Lassaigne test to get elemental analysis. Determination of the identity of unknown inorganic drugs. Determination of the identity of ten known organic and metalorganic drugs. Purification of a drug from a mixture by extraction with solvents. Qualitative analysis of drugs by UV/VIS. Spectrometry.

At the end of the course, the student will acquire the basic knowledge to carry out the identification of an unknown inorganic, organic, metallorganic drug registered in the European Official 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 the knowledge on IR and UV / Visible spectrophotometry to identify a drug.