Simultaneous fractionation of multiple classes of polyphenols from honeybush tea using solid-phase extraction

The structural diversity of polyphenols and the inherent limitations of current extraction techniques pose a challenge to extract polyphenols using a simple and green method. Hence, in this study, a method was developed to simultaneously fractionate multiple classes of polyphenols by only varying ethanol-water solutions. Honeybush tea, which is rich in polyphenols, was selected as a model for this study. Solvent extraction followed by solid-phase extraction (SPE) was developed to obtain a polyphenol-rich fraction from six honeybush samples. Based on a gradient elution programme (10%, 30%, 50%, 70% and 90% (v/v) ethanol-water solution) of SPE, the Strata X cartridge showed a better recovery of most targeted polyphenols under 0.9 mL of the drying volume and 1 mL min⁻¹ of the dispensing speed. The elution programme for fractionating most polyphenols was as follows: single elution with 50% ethanol, followed by twice elution with 70% ethanol. The antioxidant capacity was used to analyse the differences among the polyphenol-rich fractions from six honeybush samples. Principal component analysis (PCA) revealed that unfermented C. genistoides (GG) has the greatest antioxidant capacity among the honeybush species studied. Additionally, mangiferin, isomangiferin and vicenin-2 were the main contributors to the antioxidant capacity in six honeybush fractions according to the correlation study.     

Headspace fingerprinting approach to identify the major pathway influencing volatile patterns of vinasse-cured duck processed by high pressure,as well as its impact on physicochemical and sensory attributes

As a decisive attribute, flavour could be influenced by HP treatments through multiple physical and chemical pathways within the high pressure (HP)-assisted meat curing process. This investigation aimed to identify the major pathway influencing volatile flavour patterns of two representative vinasse-cured duck (VCD) products with HP treatments (150–300 MPa/15 min), including wet and dry types, by employing headspace fingerprinting as an untargeted approach. Results suggested that HP treatments greatly lowered moisture contents and increased Warner-Bratzler shear force and thiobarbituric acid reactive substances of the cured samples. According to multivariate models, the volatile flavour patterns of the HP-processed VCD could be clearly separated from the unprocessed samples, but the VCD pressurised at different intensities represented similar volatile fingerprinting, which was validated by e-nose analysis. The discriminant analysis (OPLS-DA) model outlined vinasse-derived ethanol, acetic acid, 3-methyl-1-butanol, 2-methyl-1-butanol, phenethyl alcohol and 2-methyl-3-octanone as the major discriminant aromas across the unpressurised and pressurised samples.     

Analysis of trace mercury in water by solid phase extraction using dithizone modified nanometer titanium dioxide and cold vapor atomic absorption spectrometry

A new method for analysis of trace mercury in water samples was developed, based on the combination of preconcentration/separation using dithizone-modified nanometer titanium dioxide (TiO2) as a solid phase extractant and determination by cold vapor atomic adsorption spectrometry (CVAAS). Dithizone was dissolved with alcohol and loaded on the surface of nano-sized TiO2 powders by stirring. The static adsorption behavior of Hg2 on the dithizone-modified nanoparticles was investigated in detail. It was found that excellent adsorption ratio for Hg2 could be obtained in the pH range of 7-8 with an oscillation time of 15 min, and a 5 mL of 3.5 mol·L-1 HCl solution could quantitatively elute Hg2 from nanometer TiO2 powder. Common coexisting ions caused no obvious influence on the determination of mercury. The mechanisms for the adsorption and desorption were discussed. The detection limit (3σ) for Hg2 was calculated to be 5 ng·L-1. The proposed method was applied to the determination of Hg2 in a mineral water sample and a Zhujiang River water sample. By the standard addition method, the average recoveries were found to be 94.4%-108.3% with RSD (n = 5) of 2.9%-3.5%.     

Analysis of lipid classes by solid-phase extraction and high-performance size-exclusion chromatography

An improved method to analyze lipid classes of edible oils and fats by solid-phase extraction (SPE) and high-performance size-exclusion chromatography (HPSEC) is presented. A mixture of lipid standards was fractionated by the solid-phase extraction procedure (NH₂ phase) into polar and nonpolar fractions; these were then submitted to analysis by HPSEC. The size-exclusion chromatographic columns were three styrene/divinylbenzene columns with pore sizes of 100 Å and 50 Å. Light-scattering was used for the detection system, and the parameters of the detector were optimized to minimize the difference between the responses of the compounds studied. With this procedure it was possible to separate the following lipid classes: triacylglycerols, diacylglycerols, monoacylglycerols and free fatty acids, sterols, sterol esters, tocopherols and carotenoids. Quantitative analysis was studied for a light-scattering detector with several lipid standards of different molecular weights and unsaturation levels.     

Effects of organic farming on minerals contents and aroma composition of Clemenules mandarin juice

Consumers demand organic products because they believe that the organic products are more flavorful and respectful to the environment and human health. The effects of organic farming on the minerals contents and aroma composition of Clemenules mandarin juices were studied. Minerals (Fe, Cu, Mn, Zn, Ca, Mg, K, and Na) were quantified using atomic absorption-emission spectroscopy, while volatile compounds were extracted using the dynamic headspace technique and were identified and quantified by GC–MS. In general, organic farming produced a mandarin juice with a higher quality than that produced by conventional agricultural practices. Higher concentrations of both minerals and positive volatile compounds were found in the organic juice, while the formation of off-flavors was higher in the conventional juice, although threshold values were not reached.     

The effects of harvest maturity,ripeness and storage on kiwifruit aroma

Quantitative gas chromatographic analysis of the volatile aroma components has been used as an objective measure of the effects of maturity at harvest, ripeness and storage on the aroma volatiles of kiwifruit. Increasing ripeness is associated with a rapid increase in the levels of aroma volatiles, especially esters, while increasing storage time prior to ripening is accompanied by a decrease in the amount of aroma volatiles.     

Evaluation of oxidative stability of canola oils by headspace analysis

Lipid oxidation is a major factor affecting flavor quality and shelf life of vegetable oils. Oxidative stability is therefore an important criterion by which oils are judged for usefulness in various food applications. In this study a method based on headspace analysis was developed to evaluate relative oxidative stability of canola oils. The method does not require the use of chemicals, involves minimal sample preparation, and can be performed on a relatively small sample size in comparison with traditional wet chemical methods. Canola oils freshly extracted in the laboratory from different seed samples were subjected to accelerated oxidation and analyzed for PV by standard methods and headspace volatiles by solid phase microextraction/GC-MS. Forward stepwise regression analysis of the data revealed a relationship between PV and headspace concentration of the volatile lipid oxidation products hexanal and trans,trans-2,4-heptadienal. The PV calculated using this formula correlated (R ²=0.73) with those measured by conventional methods. Presented in part at the 96th Annual Meeting of the AOCS, 1–4 May 2005, Salt Lake City, UT.     

Effect of volatiles collected above fecal pellets on behavior of the rabbit,Oryctolagus cuniculus,tested in an experimental chamber

Gas chromatographic techniques were used to trap and fractionate the volatile substances emanating from the fecal pellets of wild rabbits,Oryctolagus cuniculus, which incorporate the odor of the anal gland secretion. The volatiles were bubbled through water, trapped on Chromosorb 105, transferred to Silicone SF96 traps, passed through a GC capillary column, and retrapped on SF96. The behavioral effect of trapped and fractionated volatiles was determined in four series of bioassays involving 51 adult, male, wild-type rabbits in 112, ten-minute tests. The bioassay was based on the demonstration of territorial confidence by the rabbits under the influence of their own odor. In the bioassays of the unfractionated volatiles eluted from Chromosorb 105 and SF96 traps the animals were significantly more confident in the presence of the volatiles from their own fecal pellets. One of the two fractions of the total volatiles was ineffective while the effect of the other was less than that of the unfractionated odor. The results demonstrate that the gas chromatographic techniques can be used to manipulate complex mammalian odors with precision. Combined with a discriminative bioassay, this opens up the possibility of identifying the specific combinations of volatile substances involved in the formation of olfactory signals.     

固相萃取净化-气相色谱-质谱法测定染料中7种指示性多氯联苯

本文建立了以固相萃取(SPE)前处理净化、结合气相色谱-质谱(GC-MS)测定染料中7种指示性多氯联苯的分析方法。该法将染料样品经溶剂萃取后,通过固相萃取(SPE)净化、浓缩,气相色谱-质谱采用选择离子监测模式(SIM)测定,以保留时间和特征离子定性,外标法定量。     

Quantitation of volatile compounds in heated triolein by static headspace capillary gas chromatography/infrared spectroscopy-mass spectrometry

Static headspace and capillary gas chromatography/infrared spectroscopy-mass spectrometry were used to collect, separate, identify and quantitate the oxidative and thermal decomposition products in heated triolein. Approximately 4 L of triolein was heated in a deep-fat fryer at 190°C for 12 h each day for a total of 60 h, until it contained>-20% polymeric material. The concentration of heptane and octane increased after 12 h heating, then decreased upon further heating, while the concentration of volatile aldehydes decreased gradually during heating. After 12 h of heating, the concentrations of the major volatiles changed as follows: heptane (16.36 to 30.17 ppm), octane (24.48 to 40.77 ppm), heptanal (21.68 ppm to 9.11 ppm), octanal (35.53 to 36.64 ppm), nonanal (68.95 to 43.16 ppm), (E)-2-decenal (135.00 to 89.00 ppm) and (E)-2-undecenal (88.50 to 61.00 ppm). After 60 h of heating, when the oil contained over 20% polymeric material, the concentrations of heptane, octane, heptanal, octanol, nonanal, (E)-2-decenal and (E)-2-undecenal were 5.16, 4.39, 5.45, 7.02, 18.07, 12.50 and 6.00 ppm, respectively.