Headspace analysis of natural yoghurt using headspace solid phase microextraction : a thesis presented in partial fulfilment of the requirements for the degree of Master of Philosophy in Food Technology at Massey University (Turitea Campus), Palmerston North, New Zealand

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The Solid Phase Microextraction (SPME) method was originally developed to extract volatile and semivolatile compounds from wastewater samples but has since been applied to flavour compounds in foods and beverages. Research using the HS-SPME in related areas such as cheese and skim milk powder has been carried out but, to date, no work has been done on yoghurt flavours. The main objective of this study was to devise a methodology for the Headspace Solid Phase Microextraction (HS-SPME) technique to investigate and quantify six flavour analytes in natural, set yoghurts made from recombined milk. The relevant literature was reviewed and from it, a research proposal for this work on yoghurts was drawn. The first step in analysing and quantifying the yoghurt volatiles was to set up a working methodology for the HS-SPME method. The 100 μm polydimethylsiloxane (PDMS) fibre was chosen along with 20 minutes being the optimum fibre adsorption time. General equipment, materials and methods used throughout this thesis are also detailed. The external standard (ES) method was used to calibrate the GC and quantify the analyte concentrations in this study. The internal standard (IS) method was not used as a quantitative tool in this study. Once the HS-SPME methodology had been set up for the analysis of yoghurts, the classical Static Headspace (SH) method was compared with the HS-SPME method for extraction efficiency. The results suggested that the two methods were complementary in that the SH method extracted the more volatile compounds (acetaldehyde, acetone and 2-butanone) whereas, the HS-SPME method extracted the semi- to non-volatile compounds (ethanol, diacetyl and acetoin) more readily. However, the HS-SPME was found to be the more sensitive and effective method of the two techniques tested. The next step in the thesis was to investigate the presence of the six analytes in milk and cultured yoghurt. The effects of the sample matrix, fat levels and incubation on the volatile concentrations were also examined. The results suggested that the six analytes were inherently present in milks but at low concentrations. No conclusive effects were found for the sample matrix, fat levels and incubation. However, it was evident that fermentation of the milks using bacterial starter cultures resulted in a large increase in some of the volatiles being investigated. Following this, the effects of fat levels, storage time and storage temperature on the six volatiles in yoghurts were examined. The results indicated that significant fat level effects were only seen for diacetyl and acetoin, while temperature effects were only observed for ethanol. In both trials, only general trends for the analytes concentrations were drawn because the data varied from day to day. The results suggested that most of the compounds decreased with time except for diacetyl, which seemed to increase. The final part of this study looked at applying the devised HS-SPME methodology to a series of commercial yoghurts as a preliminary trial, with a view to investigating a potential application for the HS-SPME method. Fourteen commercial yoghurts were analysed and the six analytes quantified. The data obtained was analysed using Principle Component Analysis (PCA), which divided the yoghurts into groups based on their analyte concentrations. From these groupings, eight yoghurts were selected and fresh samples were analysed using HS-SPME and PCA. This was carried out parallel with an untrained consumer panel, which had to distinguish differences between the yoghurts in a series of triangle tests by smelling the headspace on opening the yoghurt containers. The conclusions drawn were that, unlike the HS-SPME method with PCA, the average consumer could not differentiate the yoghurts based on smell alone. PCA also showed that the HS-SPME results obtained were fairly reproducible. In conclusion, the HS-SPME method was shown to be a useful analytical technique, which can be used to analyse and quantify flavour compounds in natural, set yoghurts. This area of investigation has a lot of scope, with the results from this study providing a basis or starting point for further investigations in this area. Future studies may lead to potential applications for the HS-SPME method, one of which may be quality control where correlation of sensory data with HS-SPME analytical data is required.
Extraction (Chemistry), Analysis, Yoghurt, Flavour