Chemical Analysis of Agro-food matrices
Channel 1
ALESSANDRO D'ANNIBALE
Lecturers' profile
Program - Frequency - Exams
Course program
Analytical techniques and methods - Procedures and protocols - Concatenation of actions in the definition of an analytical problem - Guide criteria in the choice of an analytical technique - Precision - Accuracy - Required sensitivity and detection limit - Calibration and construction of a dose-signal curve - correlation diagrams - Pearson coefficient - Non-linear dose-signal relationships and transformation algorithms - Dynamic range - Preparation of standards starting from stock solutions - Signal correction strategies - Blank preparation (procedural and matrix blank solution) - External standard method - Standard addition method and unknown concentration calculation procedures - Internal standard method - Sources of errors in the analytical chain (sampling - sample preparation - analysis) - Types of matrix - Alternative sample treatment procedures - Elimination of interferents - Elimination strategies of the matrix effect (separative approaches, matrix modifiers, selective precipitation, masking methods, saturation methods and matrix matching) - Wet decomposition in an open environment - Decomposition assisted by microwave - Decomposition and for combustion - Quality control in the laboratory - Control Papers (eg. Shewhart chart and Westgart rules) - Validation of a method - Validation by comparison and correlation diagrams - Repeatability and reproducibility - Reference materials and certified reference materials (CRM) - Suppliers and CRM selection criteria - Definition and measurement of uncertainty - Horwitz equation - Compound standard uncertainty and extended uncertainty - Calculation of the LOD and LOQ - Reference parameters for the validation of a method - Measurement range - Dynamic range - Accuracy and exactness - Selectivity - Sensitivity - Robustness and solidity - Sampling - general information on errors connected to this phase - representativeness and homogeneity - integrity - Objectives and phases of a sampling - Current regulations regulating food sampling (horizontal and vertical) - Batch extraction strategies (simple, stratified or systematic randomization) Sample reduction strategies (cone and surface quarters) - Batch, sub-batch, primary sample definitions , aggregate sample, aliquot and sample unit - Examples of sampling strategies for matr Solid and liquid foodstuffs - Sampling procedures for packaged and bulk products - Sampling and sample storage devices (characteristics and materials of the containers) - Transport plan and reception procedures - Sample compliance criteria - Sampling of gases and volatile species - liquid sampling - Preparation of the laboratory sample - Determination of the number of samples to be analyzed - Chemistry laboratory - Classification of commercial chemicals - CLP regulation - GHS labeling and H and P phrases - Pictograms - Safety data sheets - Handling and storage of reagents - Water purification - deionization and reverse osmosis - glass equipment (graduated and non-graduated glassware) - devices for measuring and dispensing liquids (class A and class B) - Scales for mass measurements and associated measurement errors - Errors in measurements - Systematic and random errors - Identification and elimination of systematic errors - Treatment of random errors - Statistical parameters of dispersion - Confidence limits - Student's t - Identification of outliers - Grubbs test - Dixon test - Significance of the differences between sample means - F test - Analysis of variance - Significant figures in the measurement of quantities - Concentration expressions (molarity, formality and normality) - Preparation of solutions with known titre - Cross rule in dilutions - Extraction techniques in the liquid phase (liquid distribution - liquid: separating funnel, steam distillation, SDE extractor; liquid phase extraction under pressure - PLE solid-liquid partition: the Soxhlet system, ultrasonic or microwave extraction); solid phase extraction (SPE, SPME, Purge and Trap); extraction in supercritical (SFE) and sub-critical (ASE) phase - Nature of electromagnetic radiation - Wave and corpuscular properties of electromagnetic radiation - Energy of a photon - Interactions between radiation and matter - Energy transitions - Maxwell Boltzmann's law - Absorption - Rules selection - Emission - Fluorescence and phosphorescence - Luminescence - UV-Vis spectroscopy - Characteristic electronic transitions - Impact of the structure on the spectral behavior - Chromophores and Auxochromes - Hyperchromic and hypochromic effect - Hypsochromic and batochromic shift - Relation between absorbance and transmittance - Relation between absorbance and concentration: Lambert-Beer law - Molar extinction coefficient - Deviations from the Lambert-Beer law - Isosbestic point - UV-Vis spectrophotometers - Light sources - Monochromators with filters and dispersing elements (prism and diffraction and reflection gratings) - Interference and diffraction - Detectors - Photocells - Photomultipliers - Solid state detectors (photodiodes) - diode array detectors - Types of spectrophotometers (single beam, double beam, multi-channel) - Bandwidth of the bandwidth - Photometric resolution and linearity - Baseline stability - General applications and food analysis: pKa determination, kinetic studies, enzymatic assays - Determination of free amino acids, proteins, total and reducing sugars, fatty acids, total lipids and polyphenols
Line atomic spectra - Principles of atomic spectroscopy - Principal electronic transitions - Spectral line widening (Lorentz, Doppler effect) - Resonance wavelength - Maxwell-Boltzmann law - - Absorption, emission and fluorescence - Atomic absorption: instrumentation - Chopper and oscillating mirrors - Light sources (HCL, EDL) - Atomization techniques: Flame, Electrothermal (graphite oven), Thermal decomposition of hydrides (some elements of the IV, V and VI groups), Chemical reduction (CV, cold vapors, only for Hg), Inductively coupled plasma (ICP) - Applications to food analysis - Spectral interferences - Non-spectral interferences (chemical, physical, ionization interferences) - Interference mitigation strategies - Continuous source systems - Zeeman systems - Smith system -Hieftje - Coverage of elements by AAS - Atomic Emission Spectrometry (AES) - Inductively Coupled Plasma (ICP) - ICP-AES - ICP-MS - Quadrupole Mass Analyzers -
introduction to chromatographic methods of analysis - Solute-phase interactions - Planar and column chromatography - Classification based on the separation mechanism (Adsorption, Partition, Ion exchange, Molecular exclusion and Affinity) - Direct and inverse phase chromatography - Eluotropic series of solvents - General principles of chromatography - Distribution coefficient - capacity factor - selectivity - efficiency: HETP and number of theoretical plates - Speed theory: Van Deemter's law - Resolution - Examples of chromatographic parameters calculation - HPLC - principles - Pumping systems - injectors - columns - detectors (UV, diode-array, refractive index, ELSD, coulometric, fluorescence) - solvents and phase modifiers - isocratic and gradient elutions - HPLC-MS- ESI and ISI - HPLC applications in the agro-food sector - Gas Chromatography - Principles and Equipment - Packed Columns and Capillaries (PLOT and WCOT) - Injectors and Alternating Systems sample introduction actives - Isothermal and gradient elutions - Detectors (FID, ECD, NPD, TCD, MS) - GC applications to the agro-food sector - Electrophoresis - migration velocity and electrophoretic mobility - Titration curves of charged analytes - Vertical and horizontal electrophoretic devices - Power supplies - Ohm's law and Joule effect - Free phase electrophoresis - Zonal electrophoresis - Factors affecting resistance in anti-convective media - Paper electrophoresis - agarose and polyacrylamide gel electrophoresis - Degree of cross-linking and porosity of polyacrylamide gel - discontinuous systems and gradient gels - stroke markers and face ratio - SDS-PAGE - molecular weight determination - IEF-PAGE - determination of the isoelectric point - two-dimensional electrophoresis - Preparative electrophoresis - Protein staining (Coomassie, Silver staining) and nucleic acids (methylene blue, ethidium bromide and silver staining) - Activity staining (zymograms) - Food sector applications
Prerequisites
A good understanding of the topics covered in the course would require the possession of notions of physics and general and organic chemistry
Books
Appunti delle lezioni resi disponibili sul portale Moodle
• Harris “Chimica analitica quantitativa” ed. Zanichelli; ISBN 9788808821058
• Robinson Skelly Frame “Chimica analitica Strumentale: un'introduzione” (2023) Piccin ISBN 9788829932269
Frequency
Attendance at classes is highly recommended.
Exam mode
The final evaluation of the skills acquired by the student will be carried out through an oral interview
Lesson mode
Frontal lessons in the classroom, PPT/Inkscape presentations with schematic representations, photographs, virtual 3D objects, video, and animations. Interactive exercises in the classroom and in the chemistry lab
- Lesson code1051486
- Academic year2024/2025
- CourseFood science and technology
- CurriculumTecnologie alimentari
- Year1st year
- Semester2nd semester
- SSDAGR/13
- CFU6
- Subject areaAttività formative affini o integrative