- Docente: Anna Maria Di Pietra
- Credits: 7
- Language: Italian
- Teaching Mode: Traditional lectures
- Campus: Bologna
- Corso: Single cycle degree programme (LMCU) in Chemistry and Pharmaceutical Technologies (cod. 8412)
Learning outcomes
By following this course, the student should learn the principal identification methodologies for the drug substances, which are enlisted in the Italian and European pharmacopoeias. He could then apply the acquired knowledge to solve new analytical problems related to the pharmaceutical field.
Course contents
Drug Solubility: determination of solubility parameters; solvents; intermolecular forces: hydrogen bonding, Van der Waals and ionic interactions; structure solubility relationship, pKa of weak acid and weak base.
Liquid drugs characterizationBoiling point determination; Rault low, state diagrams; determination of relative and absolute density; refractive index determination by Abbe refractometer; qualitative analyses of liquid drugs.
Solid drugs characterization: crystal and amorphous drugs, melting point variables; crystallisation as purification method; state diagrams, eutectic mixtures, solid solutions; polymorphism.
Physical constants determination: specific optical rotatory power; polarimeter scheme and polarimetric determination.
Sample treatment, extraction methods: solvent extraction: liquid/solid extraction, liquid/liquid extraction, partition coefficient, single and multiple extraction steps. Extraction yield: pH, temperature, salts addition. Applications to pharmaceutical formulations: SPE (solid phase extraction): theory, type of sorbents, matrices with different functionalities, RAM (restricted access matrices), imprinted polymers. Extraction recovery validation; apparatus for SPE; applications to pharmaceutical formulations. SPME (solid phase microextraction) device, procedure, modus operandi. Applications to pharmaceutical formulations.
UV-VIS spectroscopy: qualitative analysis of drugs: relationship between UV spectrum profile and drug chemical structure; maximum absorption wavelength and extinction coefficient, absorbance ratio. Most important chromophores, solvent and pH effects.
Infrared spectroscopy: applications to drug analyses, identification of functional groups. Qualitative elemental analysis
Chromatographic techniques for the qualitative analysis of drugs: General concepts and criteria to choose the chromatographic technique on the basis of the drug structure; method development, optimization of chromatographic separations by variable modification; photodiode UV detection, qualitative analysis by on line UV spectra.
Qualitative elemental analysis: determination of the elements (C,N,O,S) of organic drugs; test of Lassaigne.
Identification of drugs by chemical reactivity of functional groups: alkenes, alcohols, phenols, ketones, aldehydes, acids, esters, amines, amides, nitro-derivatives and sulfur compounds.
Analytical profile of drug categories: alkaloids, amino acids, steroids, sugars, glycosides, barbiturates, xantines, penicillins, phenotiazines, benzodiazepines.
LAB Tutorials:
Qualitative identification of drug substances by chemical and instrumental methods (UV-Vis and IR spectroscopies, polarimeter, rifractometer, HPLC)
Solid phase extraction (SPE) with SAX (strong anion exchanger) matrices of ketoprofen from commercial tablets, UV analysis of the extracted analyte; liquid/liquid extraction of ephedrine and sodium benzoate in syrup; qualitative analysis of sulfamidics by HPLC-DAD.
Readings/Bibliography
V.Cavrini, V.Andrisano Principi di Analisi Farmaceutica. Esculapio, ed. 2013
Teaching methods
Theorical lessons and laboratory practice
Assessment methods
Laboratory proof and oral examination
Teaching tools
Slides, Laboratory practice
Office hours
See the website of Anna Maria Di Pietra