Malic acid or orthophosphoric acid-heat treatments for protecting sunflower (Helianthus annuus) meal proteins against ruminal degradation and increasing intestinal amino acid supply.

The protection of sunflower meal (SFM) proteins by treatments with solutions of malic acid (1 M) or orthophosphoric acid (0.67 M) and heat was studied in a 3 × 3 Latin-square design using three diets and three rumen and duodenum cannulated wethers. Acid solutions were applied to SFM at a rate of 400 ml/kg under continuous mixing. Subsequently, treated meals were dried in an oven at 150°C for 6 h. Diets (ingested at 75 g/kg BW0.75) were isoproteic and included 40% Italian ryegrass hay and 60% concentrate. The ratio of untreated to treated SFM in the concentrate was 100 : 0 in the control diet and around 40 : 60 in diets including acid-treated meals. The use of acid-treated meals did not alter either ruminal fermentation or composition of rumen contents and led to moderate reductions of the rumen outflow rates of untreated SFM particles, whereas it did not affect their comminution and mixing rate. In situ effective estimates of by-pass (BP) and its intestinal effective digestibility (IED) of dry matter (DM), CP and amino acids (AAs) were obtained considering both rates and correcting the particle microbial contamination in the rumen using 15N infusion techniques. Estimates of BP and IED decreased applying microbial correction, but these variations were low in agreement with the small contamination level. Protective treatments increased on average the BP of DM (48.5%) and CP (267%), mainly decreasing both the soluble fraction and the degradation rate but also increasing the undegradable fraction, which was higher using orthophosphoric acid. Protective treatments increased the IED of DM (108%) and CP, but this increase was lower using orthophosphoric acid (11.8%) than malic acid (20.7%). Concentrations of AA were similar among all meals, except for a reduction in lysine concentrations using malic acid (16.3%) or orthophosphoric acid (20.5%). Protective treatments also increased on average the BP of all AA, as well as the IED of most of them. Evidence of higher increases for those AA showing a high resistance to degradation in the untreated meal were also observed. The total supply of metabolisable AA was increased by 3.87 times for sulphur-containing AA, whereas that of lysine was increased by 2.5 times, mainly because of lysine losses with heat treatments. These treatments and especially that with malic acid would be useful to increase the protein value of these meals but their combined use with lysine-rich protein concentrates would improve the metabolisable protein profile.

Solid phase microextraction as a methodology in the detection of irradiation markers in ground beef.

The usefulness of solid phase microextraction (SPME) to detect the occurrence of the irradiation markers 2-dodecylcyclobutanone (2-DCB) and 1,3-bis(1,1-dimethylethyl)benzene in irradiated ground beef was evaluated. To that aim, beef samples were irradiated with different irradiation doses and subsequently examined together with non-irradiated beef samples used as control samples. The SPME conditions applied were selected as a result of performing an optimization process including different fibers (PDMS, DVB/CAR/PDMS, polyacrylate and PDMS/DVB), as well as extraction times (10, 25 and 40min) and temperatures (40 and 60°C). For comparison, 2-DCB and 1,3-bis(1,1-dimethylethyl)benzene were additionally identified in some of the samples by steam distillation-solvent extraction (SDE). Although this study is a preliminary work, from the results obtained SPME seemed to be a rapid and valuable technique to determine 2-DCB and 1,3-bis(1,1-dimethylethyl)benzene in ground beef subjected to irradiation, offering advantages over other methods reported in the literature. In addition, SPME allowed to confirm the validity of 2-DCB as an useful marker to distinguish non-irradiated from irradiated ground beef. On the contrary, the occurrence of 1,3-bis(1,1-dimethylethyl)benzene was however established in both types of samples by SPME and SDE.

Effect of thermal treatment during processing of orange juice on the enantiomeric distribution of chiral terpenes.

Chiral terpenes in orange juices were examined by solid-phase microextraction-gas chromatography-mass spectrometry to study the dependence of their enantiomeric composition on the thermal treatment applied during the industrial manufacture. The experimental conditions used in the isolation and concentration of the compounds of interest produced relative standard deviations ranging from 2.9 to 15.1% when absolute areas were used and from 1.7 to 18.3% when normalized areas were used. Recovery varied between 8.8 and 56.1%, and detection limits ranged from 0.11 to 0.32 microg/ml. The enantiomeric compositions of the majority of the chiral terpenes varied within a reasonably narrow range. Nevertheless, the enantiomeric ratio of two monoterpene alcohols, alpha-terpineol and linalool, exhibited considerable variation according to the thermal treatment used in the manufacture of the juices. Therefore, the knowledge of the enantiomeric composition of alpha-terpineol and linalool might be useful for thermal treatment control purposes.

Enantiomeric distribution of chiral compounds in orange juices according to their geographical origins.

Chiral terpenes in nonprocessed orange juices of different geographical origins were examined by two different approaches: steam distillation-solvent extraction-gas chromatography-mass spectrometry (SDE-GC-MS) and solid-phase microextraction-gas chromatography (SPME-GC). The two sample preparation techniques were compared with regard to their effectiveness in determining the enantiomeric distributions of chiral compounds. Most target compounds exhibited constant enantiomeric ratios in all juices when either of the two approaches was used. Exceptions were found for terpinen-4-ol and beta-citronellol, whose of enantiomeric purity ratios varied significantly according to the geographical origin of the sample. These results may aid in guaranteeing the authenticity and thus the quality and safety of orange juice. A comparison between the two extraction procedures revealed SPME to be more reliable for stereochemical studies, since harsh experimental conditions that can bring about racemization are not required in such studies.

Solid-phase microextraction for studies on the enantiomeric composition of filbertone in hazelnut oils.

The enantiomeric distribution of filbertone was determined in unroasted and roasted hazelnut oils of different geographical origins by using solid-phase microextraction (SPME) and capillary gas chromatography. An optimization procedure including SPME fiber, extraction time, exposure temperature, and sample volume enabled the best conditions to be selected. Under the optimized conditions, detection limits were in the micrograms per liter level for both enantiomers of filbertone with relative standard deviation values of 7.1 and 4.9% for R-filbertone and S-filbertone, respectively. The proposed approach allowed the rapid determination of the enantiomeric composition of filbertone and demonstrated that its variability is an inherent property of the natural compound. Analysis of two batches of hazelnut oils obtained from either unroasted or roasted hazelnuts showed, in general, significantly higher amounts of filbertone in roasted hazelnut oils.

Genotypic variation in fatty acid content of blackcurrant seeds.

The fatty acid composition and total fatty acid content of seeds from 36 blackcurrant genotypes developed at the Scottish Crop Research Institute were examined. A rapid small-scale procedure, involving homogenization of seeds in toluene followed by sodium methoxide transesterification and gas chromatography, was used. There was considerable variation between genotypes. The gamma-linolenic acid content generally varied from 11 to 19% of the total fatty acids, but three genotypes had higher values of 22-24%, levels previously not reported for blackcurrant seed and similar to those for borage seed. Other nutritionally important fatty acids, stearidonic acid and alpha-linolenic acid, varied from 2 to 4% and 10-19%, respectively. The mean total fatty acid contents ranged from 14 to 23% of the seed, but repeatability was poor. The results are discussed. Blackcurrant seeds are mainly byproducts from juice production, and the study shows the potential for developing blackcurrant genotypes with optimal added value.

Determination of the enantiomeric composition of gamma-lactones in edible oils by on-line coupled high performance liquid chromatography and gas chromatography.

A new method is proposed for the determination of the enantiomeric composition of gamma-lactones in different vegetable edible oils (i. e., olive oil, almond oil, hazelnut oil, peanut oil, and walnut oil), and its potential for authenticity control is underlined for a limited number of samples. The method is based on the direct injection (i.e., without requiring a sample pretreatment step) in on-line coupled reversed phase liquid chromatography to gas chromatography (RPLC-GC) using a chiral stationary phase in the GC-step. Different experimental values for both speed of sample introduction into GC and volume of the transferred fraction are considered to improve the recoveries obtained. Relative standard deviations lower than 10% and detection limits ranging from 0.06 to 0.22 mg/L were achieved for the investigated gamma-lactones.

Rapid analysis of cholesterol-elevating compounds in coffee brews by off-line high-performance liquid chromatography/high-resolution gas chromatography.

A new method is proposed to analyze the cholesterol-elevating cafestol and kahweol which allows their rapid and reliable determination in different coffee brews. The method involves the preseparation of the sample by high-performance liquid chromatography, the collection of the selected fraction, and its subsequent analysis by high-resolution gas chromatography using a programmed temperature vaporizer operated in the split mode as sampling system. Under the experimental conditions investigated, recoveries as high as 87% (cafestol) and 94% (kahweol) were achieved while detection limits equal to 0.06 and 0.04 ppm for cafestol and kahweol, respectively, were obtained. Examples are given comparing levels of cafestol and kahweol resulting from the same ground roasted coffee by different brewing methods, which show the lowest values for brews prepared from coffee bags.

Enantiomer analysis of chiral lactones in foods by on-line coupled reversed-phase liquid chromatography-gas chromatography.

A new application is proposed for the on-line coupling of reversed-phase liquid chromatography to gas chromatography (RPLC-GC) that allows the GC chirospecific analysis of gamma-lactones in fruits and commercially available fruit-containing products. The use of a programmed temperature vaporizer as an interface with the system makes the transfer of large volume fractions (i.e., 2520 microL) of aqueous eluents from LC to GC possible (speed of sample transfer, 1800 microL/min). Relative standard deviations obtained for the investigated lactones under the experimental conditions vary from 7 to 14%. The described system enlarges the LC-GC application field and overcomes the limitations reported thus far concerning the use of typical normal-phase eluents (i.e., the transfer of rather small volume fractions at low speeds of sample introduction).