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Chemometrics Methods Applied to Non-Selective Signals in Order to Address Mainly Food, Industrial and Environmental Problems

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Chemometrics Methods Applied to Non-Selective Signals in Order to Address Mainly Food, Industrial and Environmental Problems ber 2019 Decem Chemometrics Methods Applied to Non-Selective Signals in Order to Address Mainly Food, Industrial and Environmental Problems PhD Thesis Maryam Hooshyari University of Genova Doctorate in Sciences and Technologies of Chemistry and Materials Chemometrics Methods Applied to Non-Selective Signals in Order to Address Mainly Food, Industrial and Environmental Problems PhD Thesis Curriculum: SAFC XXXII Cycle Maryam Hooshyari Supervisor: Prof. Monica Casale 1 Data Sheet Title: Chemometrics Methods Applied to Non-Selective Signals in Order to Address Mainly Food, Industrial and Environmental Problems Subtitle: PhD thesis Author: Maryam Hooshyari Supervisor: Prof. Monica Casale Department: Pharmaceutical, Food and Cosmetology Sciences, Research Group of Analytical Chemistry and Chemometrics Curriculum: Pharmaceutical, Food and Cosmetology Sciences (SAFC) University: Università degli Studi di Genova Financial support: Università degli Studi di Genova Thesis Abstract: Chemometrics is a chemical discipline that uses mathematical and statistical methods in order to extract useful information from multivariate chemical data. Moreover, chemometrics is applied to correlate quality parameters or physical properties to analytical instrument data such as calculating pH from a measurement of hydrogen ion activity or a Fourier transform interpolation of a spectrum. Aim of this thesis project is to develop chemometrical strategies for the elaboration and the interpretation of non-selective complex data in order to solve real problems in food, industry and environmental fields. Keywords: Chemometrics, PCA, PARAFAC, SIMCA, PLS-CM, PLS- DA, ANOVA, PLS, QDA, D-Optimal Design, Green Tea, Lichen Thalli, Air Pollution, Engine Oil, Base Oil, Crude Oil, Naphthenic Acid, Produced Water, NIR, Fluorescence, LC- HRMS, UV-Visible, Spectroscopy, Chromatography. 2 Table of Contents Preface .......................................................................................................... 8 Chapter 1 Chemometrics Strategies in Food Projects ........................... 13 1.1 Project I D-Optimal Design and PARAFAC as Useful Tools for the Optimisation of Signals from Fluorescence Spectroscopy Prior to the Characterisation of Green Tea Sample Summary ................................................................................................. 14 1.1.1 Introduction .................................................................................... 14 1.1.2 Material and Methods .................................................................... 17 1.1.2.1 Samples and Reagents ................................................................. 17 1.1.2.2 Experimental Procedure .............................................................. 17 1.1.2.3 Instrumental ................................................................................ 18 1.1.2.4 Multivariate Data Analysis ......................................................... 18 1.1.2.4.1 PARAFAC Decomposition ...................................................... 18 1.1.2.4.2 D-Optimal Experimental Design .............................................. 19 1.1.2.5 Software ...................................................................................... 20 1.1.3 Results and Discussion ................................................................... 21 1.1.3.1 Optimization of the Procedure by Means of a D-Optimal Design .................................................................................................................. 21 1.1.3.1.1 Solid Green Tea Samples ......................................................... 21 1.1.3.1.2 Green Tea Infusions ................................................................. 26 1.1.3.2 Classification of Green Tea ......................................................... 29 1.1.3.2.1 PCA Model for Liquid Green Tea (Chinese and Indian) ......... 29 1.1.3.2.2 PCA Model for Solid Green Tea (Chinese, Japanese and Indian) .................................................................................................................. 31 1.1.3.2.3 SIMCA Model for Solid Green Tea ......................................... 34 1.1.4 Conclusions .................................................................................... 36 1.1.5 References ...................................................................................... 37 1.2 Project II Combining Excitation-Emission Matrix Fluorescence Spectroscopy, Parallel Factor Analysis, Cyclodextrin-Modified Micellar Electrokinetic 3 Chromatography and Partial Least Squares Class-Modelling for Green Tea Characterization Summary ................................................................................................. 40 1.2.1 Introduction .................................................................................... 41 1.2.2 Material and Methods .................................................................... 44 1.2.2.1 Samples and Reagents ................................................................. 44 1.2.2.2 Experimental Procedure .............................................................. 46 1.2.2.3 Instrumental ................................................................................ 46 1.2.2.3.1 Capillary Electrophoresis ......................................................... 46 1.2.2.3.2 Fluorescence Spectroscopy ...................................................... 47 1.2.2.4 Software ...................................................................................... 47 1.2.2.5 Data Analysis .............................................................................. 47 1.2.2.5.1 Data Exploration ...................................................................... 48 1.2.2.5.2 Variable Selection .................................................................... 49 1.2.2.5.3 Class Modelling ....................................................................... 49 1.2.3 Results and Discussion ................................................................... 50 1.2.3.1 Catechins and Methylxanthines Content ..................................... 50 1.2.3.2 Fluorescence Spectra ................................................................... 52 1.2.3.2.1 Repeatability Studies ................................................................ 53 1.2.3.3.2 PCA .......................................................................................... 53 1.2.3.3.3 PARAFAC ............................................................................... 55 1.2.3.3.4 Variable Selection .................................................................... 56 1.2.4 Conclusions .................................................................................... 57 Acknowledgements ................................................................................. 58 1.2.5 References ...................................................................................... 59 1.3 Project III PLS Regression Models for the Determination of EVOO Quality Parameters by NIR Spectroscopy: a Comparative Study Summary ................................................................................................. 62 1.3.1 Introduction .................................................................................... 63 1.3.2 Materials and Methods ................................................................... 65 4 1.3.2.1 Samples and Reagents ................................................................. 65 1.3.2.2 Experimental Procedure .............................................................. 66 1.3.2.3 Instrumental ................................................................................ 67 1.3.2.4 Data Analysis .............................................................................. 68 1.3.3 Result and Discussion .................................................................... 70 1.3.4 Conclusions .................................................................................... 75 Acknowledgements ................................................................................. 75 1.3.5 References ...................................................................................... 76 Chapter 2 Chemometrics Strategies in Environmental Projects .......... 78 2.1 Project IV Different analytical approaches for the biomonitoring of air pollution in Liguria region (northwest Italy) by lichens Summary ................................................................................................. 79 2.1.1 Introduction .................................................................................... 80 2.1.2 Material and Methods .................................................................... 83 2.1.2.1. Sample and Reagents ................................................................. 83 2.1.2.2. Study Area and Sampling Sites .................................................. 84 2.1.2.3 Sample Exposure ......................................................................... 84 2.1.2.4 Air Monitoring Pollution Data .................................................... 86 2.1.2.5 Instrumental ................................................................................ 86 2.1.2.5.1 Front-Face Fluorescence Spectroscopy (FFFS) ....................... 86 2.1.2.5.2 Near Infrared Spectroscopy (NIRS) ......................................... 88 2.1.2.5.3 Plant Efficiency Analyser (PEA) ............................................. 88 2.1.2.6 Data Analysis .............................................................................
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