SPME) Coupled To Gas Chromatography/mass Spectrometry Research Articles

Detection of Lard in Animal Fat Mixtures Using ATR-FTIR Fingerprint and SPME-GC/MS-Based Volatilomics

This study aims to detect the presence of lard in several halal animal fats (beef, chicken, and goat fat) based on their infrared fingerprint and volatile compound profile (volatilomics). A mixture of fat samples obtained from halal animals and lard at different concentrations (0, 20, 40, 60, and 80%, v/v) were subjected to attenuated total reflection-Fourier transformed infrared spectroscopy (ATR-FTIR) and solid phase microextraction coupled to gas chromatography-mass spectrometry (SPME-GC/MS) analysis, respectively. The data was processed using orthogonal projection to the least square–discriminant analysis (OPLS-DA). The results showed that ATR-FTIR could only identify the presence of lard in chicken fat up to the lowest concentration used in this study (10%) but failed in other fat samples. SPME-GC/MS detected the presence of lard in all animal fats up to the lowest concentration added (10%). The results of this study revealed that the volatilomics technique had more potential to be developed as a basis for the rapid detection of halal and non-halal animal fat than the infrared fingerprint. This study also emphasized that markers of non-halal animal fats can be different when the same fats are added to different food products.

Analytical Investigation of Phthalates and Heavy Metals in Edible Ice from Vending Machines Connected to the Italian Water Supply.

Edible ice is often produced by special machines that can represent a source of significant chemical and microbiological contamination. In this work, the presence of phthalic acid esters (phthalates, PAEs) and heavy metals in ice cubes distributed by 77 vending machines installed in two different zones in southern Italy and fed by water from the public water supply was investigated. Solid-phase microextraction coupled to gas chromatography-mass spectrometry (SPME-GC/MS) was used to evaluate contamination with four PAEs, which were selected because they are commonly used in the production of food-contact plastics, while inductively coupled plasma mass spectrometry (ICP/MS) was used to quantify the heavy metals. It was found that ice samples, especially those from one of the two considered zones (zone 2), exceeded the dibutyl phthalate (DBP) threshold limit value; some ice cubes from the other zone (zone 1) instead showed levels of both lead (Pb) and nickel (Ni) up to one order of magnitude higher than those observed in samples collected in zone 2 and higher than the maximum permitted values (European Directive n. 2184/2020). Since the water source connected to the ice vending machines was found to be free from significant levels of all considered target compounds and metals, the high levels of DBP, Ni, and Pb in ice cubes could be attributed to the components and/or to the state of repair of the ice vending machines themselves.

The Role of Honey Bee Derived Aliphatic Esters in the Host-Finding Behavior of Varroa destructor

Varroa destructor is an obligate ectoparasite of honey bees and shifted from its original host Apis cerana to the new host Apis mellifera in the first half of the twentieth century. The host shift has resulted in a great threat to the health and survival of A. mellifera colonies worldwide. Chemical signals play a crucial role in all aspects of the Varroa life cycle, including host finding. However, the chemical cues that affect the host finding behavior of Varroa mites are still not fully understood. In this study, we systematically profiled the headspace volatiles of both worker and drone larvae of the two honey bee species by using solid phase micro-extraction coupled to gas chromatography-mass spectrometry (SPME-GC-MS), and then used electrophysiological recording and Y-tube olfactometer bioassay to study the potential roles of the selected compounds. The chemical profiling showed that there were four aliphatic esters, ethyl myristate (EM), methyl palmitate (MP), ethyl palmitate (EP), and ethyl oleate (EO) commonly detected from all four types of larval hosts. Among them, EM was a new substance identified from honey bee headspace volatiles. Results from electrophysiological recordings indicated that all the aliphatic esters could elicit significant responses of Varroa pit organs on its forelegs. Moreover, behavioral analyses revealed that EM could significantly attract V. destructor at a medium dosage (10 µg), while MP had no observable effect on the mites and both EP and EO were able to repel the parasites. Our findings suggest an important role of host-derived aliphatic esters in Varroa host finding, and provide new chemicals for Varroa monitoring and control.

Volatile Organic Compounds (VOCs) Produced by Gluconobacter cerinus and Hanseniaspora osmophila Displaying Control Effect against Table Grape-Rot Pathogens.

Table grapes (Vitis vinifera) are affected by botrytis bunch rot and summer bunch rot, the latter a complex disease caused by Botrytis cinerea, Aspergillus spp., Penicillium expansum and Rhizopus stolonifer. To search for biocontrol alternatives, a new bioproduct composed of Gluconobacter cerinus and Hanseniaspora osmophila, a consortium called PUCV-VBL, was developed for the control of fungal rots in table grapes. Since this consortium presents new biocontrol species, the effect of their VOCs (volatile organic compounds) was evaluated under in vitro and in vivo conditions. The VOCs produced by the PUCV-VBL consortium showed the highest mycelial inhibition against Botrytis cinerea (86%). Furthermore, H. osmophila was able to inhibit sporulation of A. tubingensis and P. expansum. VOCs’ effect in vivo was evaluated using berries from Red Globe, Thompson Seedless and Crimson Seedless grapes cultivars, demonstrating a mycelial inhibition by VOCs greater than 70% for all evaluated fungal species. The VOC identification of the PUCV-VBL consortium was analyzed by solid-phase microextraction coupled to gas chromatography-mass spectrometry (SPME-GCMS). A total 26 compounds were identified, including 1-butanol 3-methyl, propanoic acid ethyl ester, ethyl acetate, phenylethyl alcohol, isobutyl acetate and hexanoic acid ethyl ester. Our results show that VOCs are an important mode of action of the PUCV-VBL biological consortium.

Fabrication of montmorillonite/ionic liquid composite coated solid-phase microextraction fibers for determination of phenolic compounds in fruit juices by gas chromatography and liquid chromatography

Novel montmorillonite composites including ionic liquid were prepared and utilized as coating materials for solid phase microextraction fibers. Ionic liquids containing amino terminated imidazolium cations with methyl and benzyl groups and hydrophobic anions (bis(trifluoromethylsulfonyl)imide) and hydrophilic anions (bromide and tetrafluoroborate) were intercalated to KSF-montmorillonite using stainless steel wire as support by using the layer-by-layer technique. After optimization of experimental conditions, solid phase microextraction (SPME) coupled to gas chromatography/mass spectrometry (SPME-GC/MS) after derivatization by silylation and high performance liquid chromatography/diode array detector (SPME-HPLC/DAD) were developed for the determination of 16 phenolic compounds. The developed SPME-GC/MS method had wider linearity and lower limit of detection than the developed SPME-HPLC/DAD method with similar repeatability (for 5 runs, less than 4.2 %) for a single fiber. The percentage of the variance between two different fibers was less than 6.0 % in both methods. The developed SPME methods were applied successfully to fresh fruit juices and the relative recoveries and the repeatabilities from spiked fruit juice samples were satisfactorily achieved. The results obtained with both chromatographic methods were in good agreement with each other.

Geographical traceability of Italian white truffle (Tuber magnatum Pico) by the analysis of volatile organic compounds

Results are presented that were obtained on the geographic traceability of the white truffle Tuber magnatum Pico. Solid-phase microextraction coupled to gas chromatography/mass spectrometry (SPME-GC/MS) was employed to characterize the volatile profile of T. magnatum white truffle produced in seven geographical areas of Italy. The main components of the volatile fraction were identified using SPME-GC/MS. Significant differences in the proportion of volatile constituents from truffles of different geographical areas were detected. The results suggest that, besides genetic factors, environmental conditions influence the formation of volatile organic compounds. The mass spectra of the volatile fraction of the samples were used as fingerprints to characterize the geographical origin. Next, stepwise factorial discriminant analysis afforded a limited number of characteristic fragment ions that allowed a geographical classification of the truffles studied.

Solid phase microextraction coupled to gas chromatography- mass spectrometry for the determination of the adsorption coefficients of triazines in soil

Solid phase microextraction coupled to gas chromatography-mass spectrometry (SPME-GC-MS) was used to determine the adsorption coefficients (Koc) for six target triazines in soil and sediment samples with different organic matter contents and textures. SPME-GC-MS was used in conjunction with a conventional batch equilibrium method. The recoveries of the selected triazines from soils and sediments having organic carbon contents in the range 0.2–2.4% were satisfactory. Drawbacks of conventional analytical techniques are avoided; owing to the selectivity of SPME-GC-MS, no sample pre-treatment or solvent enrichment steps were required so that Koc values could be easily determined. Moreover, the sensitivity of the technique makes it possible to work at low triazine concentrations (50–500 ng g–1) where the Freundlich adsorption isotherm can be considered linear.