Application of chromatographic and spectroscopic techniques in the evaluation of the lipid fraction of animal products

Lipolysis and oxidation of lipids in foods are the major biochemical and chemical processes that cause food quality deterioration, leading to the characteristic, unpalatable odour and flavour called rancidity. In addition to unpalatability, rancidity may give rise to toxic levels of certain compounds like aldehydes, hydroperoxides, epoxides and cholesterol oxidation products. In this PhD study chromatographic and spectroscopic techniques were employed to determine the degree of rancidity in different animal products and its relationship with technological parameters like feeding fat sources, packaging, processing and storage conditions. To achieve this goal capillary gas chromatography (CGC) was employed not only to determine the fatty acids profile but also, after solid phase extraction, the amount of free fatty acids (FFA), diglycerides (DG), sterols (cholesterol and phytosterols) and cholesterol oxidation products (COPs). To determine hydroperoxides, primary products of oxidation and quantify secondary products UV/VIS absorbance spectroscopy was applied. Most of the foods analysed in this study were meat products. In actual fact, lipid oxidation is a major deterioration reaction in meat and meat products and results in adverse changes in the colour, flavour and texture of meat. The development of rancidity has long recognized as a serious problem during meat handling, storage and processing. On a dairy product, a vegetal cream, a study of lipid fraction and development of rancidity during storage was carried out to evaluate its shelf-life and some nutritional features life saturated/unsaturated fatty acids ratio and phytosterols content. Then, according to the interest that has been growing around functional food in the last years, a new electrophoretic method was optimized and compared with HPLC to check the quality of a beehive product like royal jelly. This manuscript reports the main results obtained in the five activities briefly summarized as follows: 1) comparison between HPLC and a new electrophoretic method in the evaluation of authenticity of royal jelly; 2) study of the lipid fraction of a vegetal cream under different storage conditions; 3) study of lipid oxidation in minced beef during storage under a modified atmosphere packaging, before and after cooking; 4) evaluation of the influence of dietary fat and processing on the lipid fraction of chicken patties; 5) study of the lipid fraction of typical Italian and Spanish pork dry sausages and cured hams.

Development and characterization of a distributed measurement system for the evaluation of voltage quality in electric power networks

The research activity carried out during the PhD course in Electrical Engineering belongs to the branch of electric and electronic measurements. The main subject of the present thesis is a distributed measurement system to be installed in Medium Voltage power networks, as well as the method developed to analyze data acquired by the measurement system itself and to monitor power quality. In chapter 2 the increasing interest towards power quality in electrical systems is illustrated, by reporting the international research activity inherent to the problem and the relevant standards and guidelines emitted. The aspect of the quality of voltage provided by utilities and influenced by customers in the various points of a network came out only in recent years, in particular as a consequence of the energy market liberalization. Usually, the concept of quality of the delivered energy has been associated mostly to its continuity. Hence the reliability was the main characteristic to be ensured for power systems. Nowadays, the number and duration of interruptions are the “quality indicators” commonly perceived by most customers; for this reason, a short section is dedicated also to network reliability and its regulation. In this contest it should be noted that although the measurement system developed during the research activity belongs to the field of power quality evaluation systems, the information registered in real time by its remote stations can be used to improve the system reliability too. Given the vast scenario of power quality degrading phenomena that usually can occur in distribution networks, the study has been focused on electromagnetic transients affecting line voltages. The outcome of such a study has been the design and realization of a distributed measurement system which continuously monitor the phase signals in different points of a network, detect the occurrence of transients superposed to the fundamental steady state component and register the time of occurrence of such events. The data set is finally used to locate the source of the transient disturbance propagating along the network lines. Most of the oscillatory transients affecting line voltages are due to faults occurring in any point of the distribution system and have to be seen before protection equipment intervention. An important conclusion is that the method can improve the monitored network reliability, since the knowledge of the location of a fault allows the energy manager to reduce as much as possible both the area of the network to be disconnected for protection purposes and the time spent by technical staff to recover the abnormal condition and/or the damage. The part of the thesis presenting the results of such a study and activity is structured as follows: chapter 3 deals with the propagation of electromagnetic transients in power systems by defining characteristics and causes of the phenomena and briefly reporting the theory and approaches used to study transients propagation. Then the state of the art concerning methods to detect and locate faults in distribution networks is presented. Finally the attention is paid on the particular technique adopted for the same purpose during the thesis, and the methods developed on the basis of such approach. Chapter 4 reports the configuration of the distribution networks on which the fault location method has been applied by means of simulations as well as the results obtained case by case. In this way the performance featured by the location procedure firstly in ideal then in realistic operating conditions are tested. In chapter 5 the measurement system designed to implement the transients detection and fault location method is presented. The hardware belonging to the measurement chain of every acquisition channel in remote stations is described. Then, the global measurement system is characterized by considering the non ideal aspects of each device that can concur to the final combined uncertainty on the estimated position of the fault in the network under test. Finally, such parameter is computed according to the Guide to the Expression of Uncertainty in Measurements, by means of a numeric procedure. In the last chapter a device is described that has been designed and realized during the PhD activity aiming at substituting the commercial capacitive voltage divider belonging to the conditioning block of the measurement chain. Such a study has been carried out aiming at providing an alternative to the used transducer that could feature equivalent performance and lower cost. In this way, the economical impact of the investment associated to the whole measurement system would be significantly reduced, making the method application much more feasible.

Monitoring of New Psychoactive Substances in the hair of patients with a history of addiction. Evaluation of the public health impact.

Introduction. The term New Psychoactive Substances (NPS) encompasses a broad category of drugs which have become available on the market in recent years and whose illicit use for recreational purposes has recently exploded. The analysis of NPS usually requires mass spectrometry based techniques. The aim of our study was to define the preva-lence of NPS consumption in patients with a history of drug addiction followed by Public Services for Pathological Addictions, with the purpose of highlighting the effective presence of NPS within the area of Bologna and evaluating their association with classical drugs of abuse (DOA). Materials and methods. Sustained by literature, a multi-analyte UHPLC-MS/MS method for the identification of 127 NPS (phenethylamines, arylcyclohexylamines, synthetic opioids, tryptamines, synthetic cannabinoids, synthetic cathinones, designer benzodiazepines) and 15 classic drugs of abuse (DOA) in hair samples was developed and validated according to International Guidelines [112]. Samples pretreatment consisted of washing steps and overnight incubation at 45°C in an acid mixture of methanol and water. After cooling, supernatant were injected into the chromatographic system coupled with a tandem mass spectrometry detector. Results. Successful validation was achieved for almost all of the compounds. The method met all the required technical parameters. LOQ was set from 4 to 80 pg/mg The developed method was applied to 107 cases (85 males and 22 females) of clinical interest. Out of 85 hair samples resulting positive to classical drugs of abuse, NPS were found in twelve (8 male and 4 female). Conclusion. The present methodology represents an easy, low cost, wide-panel method for the de-tection of 127 NPS and 15 DOA in hair samples. Such multi-analyte methods facilitates the study of the prevalence of drugs abused that will enable the competent control authorities to obtain evi-dence-based reports regarding the critical spread of the threat represented by NPS.