Measurement of caffeine in coffee beans with UV/vis spectrometer

In this research work using UV/vis spectrophotometer the molar decadic absorption coefficients and transitional dipole moment of pure caffeine in water and dichloromethane were obtained at 272 and 274.7 nm. The molar decadic absorption coefficients of caffeine in water and dichloromethane at these wavelengths are 1115 and 1010 m² mol⁻¹, respectively. The calculated values for the transitional dipole moment of caffeine in water and in dichloromethane are 10.40 × 10⁻³⁰ and 10.80 × 10⁻³⁰ C m, respectively. After characterizing caffeine in water and dichloromethane, fast and simple methods were developed that enable to quantify the content of caffeine in coffee beans. The methods helped in extracting caffeine from coffee dissolved in water by dichloromethane, and Gaussian fit was applied to eliminate the possible interference with the caffeine spectra.     

Structural and chromatic characterization of a new Malvidin 3-glucoside–vanillyl–catechin pigment

A new pigment, resulting from the reaction between malvidin 3-glucoside and catechin in the presence of vanillin, was detected in a model solution. This newly formed anthocyanin-aryl-flavanol adduct was structurally characterized by 1D and 2D NMR and mass spectrometry, and its chromatic characteristics were studied by UV–Vis techniques. The new pigment was shown to have a wavelength of maximum absorption in the visible region (λ_max) of 549 nm, conferring on it a purple colour, and a molar extinction coefficient value (ε) of 12,247 l · mol⁻¹ · cm⁻¹.     

Analysis of some selected catechins and caffeine in green tea by high performance liquid chromatography

Green tea seems to have a positive impact on health due to the catechins-found as flavanols. Thus, the present study was aimed to develop a low cost reversed phase high performance liquid chromatographic (HPLC) method for simultaneous determination of flavanol contents, namely catechin (C), epicatechin (EC), epigallocatechin (EGC), epicatechin 3-gallate (ECG) and epigallocatechin 3-gallate (EGCG) and caffeine in 29 commercial green tea samples available in a Saudi Arabian local market. A C-18 reversed-phase column, acetonitrile–trifluoroacetic acid as a mobile phase, coupled with UV detector at 205 nm, was successfully used for precise analysis of the tested analytes in boiled water of digested tea leaves. The average values of N (No. of theoretical plates), HETP (height equivalent of theoretical plates) and R_s (separation factor) (at 10 μg ml⁻¹ of the catechins EC, EGC, EGCG and ECG) were 2.6 × 10³ ± 1.2 × 10³, 1.7 × 10⁻³ ± 4.7 × 10⁻⁴ cm and 1.7 ± 5.53 × 10⁻², respectively. The developed HPLC method demonstrated excellent performance, with low limits of detection (LOD) and quantification (LOQ) of the tested catechins of 0.004–0.05 μg ml⁻¹ and 0.01–0.17 μg ml⁻¹, respectively, and recovery percentages of 96–101%. The influence of infusion time (5–30 min) and temperature on the content of the flavanols was investigated by HPLC. After a 5 min infusion of the tea leaves, the average concentrations of caffeine, catechin, EC, EGC, ECG and EGCG were found to be in the ranges 0.086–2.23, 0.113–2.94, 0.58–10.22, 0.19–24.9, 0.22–13.9 and 1.01–43.3 mg g⁻¹, respectively. The contents of caffeine and catechins followed the sequence: EGCG > EGC > ECG > EC > C > caffeine. The method was applied satisfactorily for the analysis of (+)-catechin, even at trace and ultra trace concentrations of catechins. The method was rapid, accurate, reproducible and ideal for routine analysis.     

Interaction of milk α- and β-caseins with tea polyphenols

The interaction of α- and β-caseins with tea polyphenols (+)-catechin (C), (−)-epicatechin (EC), (−)-epigallocatechin (EGC) and (−)-epigallocatechin gallate (EGCG) was examined at a molecular level, using FTIR, UV–visible, CD and fluorescence spectroscopic methods as well as molecular modelling. The polyphenol binding mode, the binding constant and the effects of polyphenol complexation on casein stability and conformation were determined. Structural analysis showed that polyphenols bind casein via both hydrophilic and hydrophobic interactions with overall binding constants of K_C–α-cas = 1.8 (±0.8) × 10³ M⁻¹, K_EC–α-cas = 1.8 (±0.6) × 10³ M⁻¹, K_EGC–α-cas = 2.4 (±1.1) × 10³ M⁻¹ and K_{EGCG–α-cas} = 7.4 (±0.4) × 10³ M⁻¹, K_C–β-cas = 2.9 (±0.3) × 10³ M⁻¹, K_EC–β-cas = 2.5 (±0.6) × 10³ M⁻¹, K_EGC–β-cas = 3.5 (±0.7) × 10³ M⁻¹ and K_{EGCG–β-cas} = 1.59 (±0.2) × 10⁴ M⁻¹. The number of polyphenol bound per protein molecule (n) was 1.1 (C), 0.9 (EC), 1.1 (EGC), 1.5 (EGCG) for α-casien and 1.0 (C), 1.0 (EC), 1.1 (EGC) and 1.5 (EGCG) for β-casein. Structural modelling showed the participation of several amino acid residues in polyphenol–protein complexation with extended H-bonding network. Casein conformation was altered by polyphenol with a major reduction of α-helix and β-sheet and increase of random coil and turn structure suggesting further protein unfolding. These data can be used to explain the mechanism by which the antioxidant activity of tea compounds is affected by the addition of milk.     

Assessment and validation of methods for the determination of γ-glutamyltransferase activity in sheep milk

The determination of enzymatic activity in sheep milk is still today a practically unexplored field of research. This study proposes and fully validates two analytical procedures (i.e. by means of UV–vis spectrophotometry and RP-HPLC methods) for the determination of γ-glutamyltransferase activity in sheep milk. Both methods are characterised by low detection and quantification limits, excellent linearity over a wide enzymatic activity interval, very good repeatability and reproducibility, and are bias-free. The RP-HPLC method provides better sensitivity and automation capability levels than that of UV–vis, and its use is hence suggested for screening purposes. These methods have been preliminarily tested with a number of real samples of whole sheep milk, obtaining an average γ-glutamyltransferase activity value of 2.93 ± 0.50 U ml⁻¹ and a range from 2.72 ± 0.10 U ml⁻¹ to 3.46 ± 0.11 U ml⁻¹.     

Solid phase extraction with flame atomic absorption spectrometry for determination of traces of Ca,K, Mg and Na in quality control of white sugar

A fast and straightforward pre-concentration procedure based on solid phase extraction with a strongly acidic cation-exchanger Dowex 50 W × 8–400 was proposed to determine traces of Ca, K, Mg and Na in white sugar samples by means of flame atomic absorption spectrometry. For this purpose, 20% (m/v) white sugar solutions (100 ml) were driven through resin beds at 10 ml min⁻¹ to retain Ca, K, Mg and Na ions and to separate sucrose that passed through unretained. Thereafter, columns were rinsed with water and elements of interest were recovered prior to measurements using 5 ml of a 2 mol l⁻¹ HCl solution. Detection limits of 0.04, 0.05, 0.02 and 0.01 μg g⁻¹ for Ca, K, Mg and Na, respectively, and precision of measurements within 1–3% were achieved. The proposed method enabled to determine Ca, K, Mg and Na in samples of white sugar within corresponding ranges: 0.66–0.99 μg g⁻¹ (Ca), 2.9–12.2 μg g⁻¹ (K), 0.53–1.57 μg g⁻¹ (Mg) and 0.06–0.30 μg g⁻¹ (Na). Accuracy of this sample pre-treatment procedure and analysis method was assessed by performing spikes and recovery experiments. Recoveries of added Ca, K, Mg and Na were found to be within 97–102%, demonstrating good reliability of results.     

Iron-chelation properties of phenolic acids bearing catechol and galloyl groups

In this study, the capacity of seven phenolic acids and hydroxytyrosol for complex formation with iron was quantified. A metal-chelation mechanism was described by means of spectrophotometry and calculating the binding constants of the complexes. The influence of phosphate buffer, Hepes buffer, Tris buffer and water on this mechanism was investigated. UV–Vis absorption spectroscopy showed that the absorption of phenolic acids changes upon the addition of Fe²⁺, which resulted in several shifts of their spectra. These batochromic shifts were analyzed and evaluated by calculating binding constants. Furthermore, in the presence of different concentrations of EDTA (0–1 mM), a reduction of the constants was observed. However, not all of the phenolic compounds assessed here showed complex formation, those not bearing catechol or galloyl moiety like vanillic acid, syringic acid and ferulic acid, did not show any complex formation in our study. The ability of the phenolic compounds which chelate iron have been ranked in line with the binding constants in ascending order rendering the protocatechuic acid (1.43 M⁻¹) the weakest chelator, followed by hydroxytyrosol (2.66 M⁻¹), gallic acid (4.78 M⁻¹), caffeic acid (8.12 M⁻¹) and chlorogenic acid (20.13 M⁻¹) as the strongest chelator.     

Biodegradable three-layer film derived from bovine gelatin

Biodegradable three-layer gelatin film was obtained by heat – compression of piled dialdehyde starch (DAS) – cross-linked and plasticized-gelatin films (Ge-10DAS) outer layers and sodium montmorillonite (MMt) – plasticized – gelatin film (Ge-5MMt) inner layer. Multilayer film displayed a compact and uniform microstructure due to the highly compatible individual layers which could interact by strong hydrogen bonding. Lamination reduced moisture absorption and total soluble matter compared to the single layers while keeping transparency. Tensile strength and elastic modulus of the multilayer were 8.0 ± 1.3 MPa and 14.7 ± 2.4 MPa, which were significantly higher than values obtained for Ge-10DAS due to the contribution of the of the bio-nanocomposite inner layer. Elongation at break was not affected by lamination meanwhile it had a beneficial effect on barrier properties. Water vapor permeability (WVP) of the multilayer was 0.8 ± 0.1 × 10⁻¹³ kg m Pa⁻¹ s⁻¹ m⁻² which was lower than those of the individual components whereas oxygen permeability was similar to that of Ge-5MMt (10.5 ± 0.4 cm³(O₂) mm m⁻² day⁻¹) and lower than that of Ge-10DAS film.     

Fingerprint of enological tannins by multiple techniques approach

In this study, six enological tannins (T1–T6) from different source were analysed by selected analytical techniques, including UV–Vis, FTIR, NMR, SEC, LC-MS/MS and electronic nose. Moreover, the samples were tested for their antioxidant activity. Spectra and chromatograms are considered as a fingerprint with a pattern that is distinctive for a given type of sample. In particular, tannins showed the maximum UV–Vis absorbance (λ_max) at 273–280 nm, the inflection point (λ_min) at 247–264 nm, and the ratio λ_max/λ_min was 1.03, 1.35, 1.67, 1.36, 2.15, 2.02 for tannin T1–T6, respectively. The FTIR analysis of tannins showed the presence of most important absorption bands at 1522, 1453, 1380, 1350, 1328, 1286, 1210, 1148 and 1044 cm⁻¹. Besides, SEC and NMR analysis allowed to sort the tannins according to their average DP as follows: T1 > T2 = T4 > T3 > T6 = T5. Based on this multiple techniques approach three condensed tannins (sample T3, T5 and T6) were clearly identified, together with two mixtures of hydrolysable tannins (sample T1 and T2), whereas one sample (T4) showed a peculiar pattern different from the commercial tannin commonly used in enology.     

Folic acid complexes with human and bovine serum albumins

The interaction of folic acid with human serum (HSA) and bovine serum albumins (BSA) at physiological conditions, using constant protein concentration and various folic acid contents was investigated. FTIR, UV–visible and fluorescence spectroscopic methods as well as molecular modelling were used to analyse folic acid binding sites, the binding constant and the effect on HSA and BSA stability and conformations. Structural analysis showed that folic acid binds HSA and BSA via both hydrophilic and hydrophobic contacts with overall binding constants of K_{folic acid–HSA} = 8.1 (±0.5) × 10⁴ M⁻¹ and K_{folic acid–BSA} = 1.0 (±0.3) × 10⁵ M⁻¹. The number of bound acid molecules per protein was 1.7 (±0.4) for HSA and 1.5 (±0.3) for BSA complexes. Molecular modelling showed participation of several amino acids in folic acid–protein complexes stabilised by hydrogen bonding network. Folic acid complexation altered protein secondary structure by major reduction of α-helix from 59% (free HSA) to 35% (acid-complex) and 62% (free BSA) to 25% (acid-complex) with an increase in random coil, turn and β-sheet structures indicating protein unfolding. The results suggest that serum albumins might act as carrier proteins for folic acid in delivering it to target molecules.     

Migration of α-tocopherol and resveratrol from poly(L-lactic acid)/starch blends films into ethanol

Poly(L-lactic acid) (PLLA)/starch blends with various concentrations of two natural antioxidants, α-tocopherol (α-TOC) and resveratrol, were fabricated by a melt blending and compression molding processes. The effects of the two antioxidants on the optical (color), thermal and mechanical properties of PLLA/starch blends with antioxidants were assessed. PLLA/starch blend films with α-TOC and resveratrol showed a yellowish color influenced by the combined effect of white starch and the brown color of the antioxidants. The glass transition and melting temperatures were significantly reduced with the addition of antioxidants while enhanced thermal stability was observed, which could be a benefit and important for processing and production. The enhanced mechanical properties could be attributed to not only a compatibilization effect based on the chemical linkage between PLLA and starch chains, but also restriction of the chain mobility by antioxidants. The release of resveratrol from PLLA and PLLA/starch blend films into ethanol followed Fickian behavior. The D values of α-TOC were in the range of 0.47–3.95 × 10⁻¹¹ cm² s⁻¹ for PLLA films and 0.70–6.83 × 10⁻¹¹ cm² s⁻¹ for PLLA/starch blend films at 13 °C, 5.67–13.0 × 10⁻¹¹ cm² s⁻¹ for PLLA films and 4.10–24.2 × 10⁻¹¹ cm² s⁻¹ for PLLA/starch blend films at 23 °C, and 89.0–118.0 × 10⁻¹¹ cm² s⁻¹ for PLLA films and 123–282 × 10⁻¹¹ cm² s⁻¹ for PLLA/starch blend films at 43 °C. The D values of resveratrol were in the range of 0.073–0.54 × 10⁻¹⁰ cm² s⁻¹ for PLLA films and 1.42–6.93 × 10⁻¹⁰ cm² s⁻¹ for PLLA/starch blend films at 13 °C, 0.90–3.44 × 10⁻¹⁰ cm² s⁻¹ for PLLA films and 4.16–22.3 × 10⁻¹⁰ cm² s⁻¹ for PLLA/starch blend films at 23 °C, and 24.8–74.1 × 10⁻¹⁰ cm² s⁻¹ for PLLA films and 40.1–309 × 10⁻¹⁰ cm² s⁻¹ for PLLA/starch blend films at 43 °C.     

Chlorogenic acid and caffeine contents in various commercial brewed coffees

Twelve commercial brewed coffees (seven regular and five decaffeinated) were analyzed for chlorogenic acids (CGA) and caffeine by HPLC. Their pH and UV–Vis absorbances were also measured. The CGAs identified were three caffeolylquinic acids (3-CQA, 4-CQA, and 5-CQA), three feruloylquinic acids (3-FQA, 4-FQA, and 5-FQA), and three dicaffeoylquinic acids (3,4-diCQA, 3,5-diCQA, and 4,5-diCQA). The total CGAs ranged from 5.26 mg/g to 17.1 mg/g in regular coffees and from 2.10 mg/g to 16.1 mg/g in decaffeinated coffees. Among CGA, 5-CQA was present at the highest level, ranging from 2.13 mg/g to 7.06 mg/g coffee, and comprising 36–42% and 37–39% of the total CGA in the regular and decaffeinated coffees, respectively. CGA isomer contents were, in decreasing order, 5-CQA > 4-CQA > 3-CQA > 5-FQA > 4-FQA > 3-FQA > 3,4-diCQA > 4,5-diCQA, 3,5-diCQA. The caffeine content in regular and decaffeinated coffees ranged from 10.9 mg/g to 16.5 mg/g and from 0.34 mg/g to 0.47 mg/g, respectively. The pH of regular and decaffeinated coffees ranged from 4.95 to 5.99 and from 5.14 to 5.80, respectively. The relationship between the pH and the UV–Vis absorbance at 325 nm was moderately correlated (R² = 0.7829, p < 0.001, n = 12).     

Synthesis and application of a new functionalized resin for use in an on-line,solid phase extraction system for the determination of trace elements in waters and reference cereal materials by flame atomic absorption spectrometry

The synthesis and characterization of the resin Amberlite XAD-4 functionalized with 2,6-pyridinedicarboxaldehyde and its application in an on-line system for the preconcentration of cadmium, cobalt, copper, lead and manganese prior to determination using flame atomic absorption spectrometry (FAAS) is proposed. Metal ions retained on the modified resin were eluted using 1.0 mol L⁻¹ HNO₃ solution and aspirated directly to the nebulizer–burner system of a FAAS instrument using a flow injection system. Detection limits (3σ) were determined to be 0.13 μg L⁻¹ for Cd, 0.29 μg L⁻¹ for Cu, 0.23 μg L⁻¹ for Mn, 0.58 μg L⁻¹ for Co and 2.19 μg L⁻¹ for Pb using a 10 mL of water sample loading volume. The limits of detection would be 100 times higher with units of μg kg⁻¹ for the solid samples in which their dilution ratios as (volume/weight) were 100. Enrichment factors ranged from 23.6 to 28.9 (for Co and Mn, respectively). The proposed method was successfully applied to determination of the analytes in natural water samples and certified reference materials.     

Analysis of potential adulteration in herbal medicines and dietary supplements for the weight control by capillary electrophoresis

Four different phytopharmaceutical dosage forms for use in weight control programs were analyzed. Two different ground herbal blends and their correspondent infusions, a capsule and a tincture were investigated for the presence of compounds used as adulterants in these products. A capillary electrophoresis (CE) method was developed and validated. The optimized experimental conditions were: BGE, sodium tetraborate buffer 20 mM, pH 9.2, voltage applied 30 kV, capillary temperature 25 °C, injection sample at 0.5 Psi during 5 s. Ephedrine, norephedrine, caffeine and furosemide were baseline separated in less than 7 min; the migration times were found to be 2.65, 2.90, 3.75 and 6.58 min, respectively. The analysis showed in sample 3 concentrations of 0.45 ± 0.03 mg g⁻¹ (ephedrine), 0.33 ± 0.02 mg g⁻¹ (norephedrine), 1.09 ± 0.41 mg g⁻¹ (caffeine) and 0.80 ± 0.17 mg g⁻¹ (furosemide). Caffeine content in samples 1, 2 and 4 was 0.61 ± 0.06 mg g⁻¹, 15.66 ± 1.05 mg g⁻¹ and 2.27 ± 0.13 mg ml⁻¹, respectively. Linearity was obtained in the concentration range of 1–1000 μg ml⁻¹. Limits of detection (LOD) and quantification (LOQ) were determined as 0.42 μg ml⁻¹ and 1.40 μg ml⁻¹ (ephedrine), 0.47 μg ml⁻¹ and 1.40 μg ml⁻¹ (norephedrine), 0.12 μg ml⁻¹ and 0.48 μg ml⁻¹ (caffeine), 0.22 μg ml⁻¹ and 0.73 μg ml⁻¹ (furosemide).     

Determination of polycyclic aromatic hydrocarbons in edible oils and barbecued food by HPLC/UV–Vis detection

Determination of nine polycyclic aromatic hydrocarbons in corn, sunflower, olive oils and barbecued meat and fish by HPLC/UV–Vis method is described. The extraction procedure included a saponification, liquid–liquid extraction and finally purification of PAHs through a house-made silica–alumina column. Chromatographic determination was based on separation of PAHs on ODS column and measurement at 254 nm. All polycyclic aromatic hydrocarbons were separated and analyzed in 12 min on reversed phase ODS column with acetonitrile/water mobile phase at 1.5 mL min⁻¹ flow rate. The detection limits of nine polycyclic aromatic hydrocarbons ranged from 0.26 to 1.15 μg L⁻¹ at a signal/noise ratio of 3. The linearity of the method was between 0.9951 and 0.9996. Oil samples contain different PAHs ranging from 0.44 to 98.92 μg L⁻¹. Barbecuing process increased the concentration (in the range of 2- to 8-fold) and caused the formation of PAHs in food samples.     

Selenium species in buckwheat cultivated with foliar addition of Se(VI) and various levels of UV-B radiation

Common (Fagopyrum esculentum Moench) and tartary (Fagopyrum tataricum Gaertn.) buckwheat was treated by spraying the leaves with a water solution containing 15 mg Se per litre in the form of sodium selenate in the flowering period. The selenium content in all parts of plant was found to be less than 200 ng g⁻¹ in non-treated and in the range 2700–4650 ng g⁻¹ in selenium treated buckwheat. Exposure to UV-B radiation lead to higher Se accumulation in flowers of both Se enriched cultivars. For speciation analysis enzymatic hydrolysis was carried out, separation and detection of selenium species was performed by high performance liquid chromatography–ultraviolet treatment–hydride generation atomic fluorescence spectrometry (HPLC–UV–HG-AFS). In flowers and leaves, on average 11% of the Se content was soluble and in the form of Se(VI), representing between 0.6% (flowers) and 3% (leaves) of the Se content. The remaining soluble non-amino acid organic Se was not detected by HPLC–UV–HG-AFS. In seeds 93% of the selenium content was found in the extracts and the main selenium species was SeMet with 93 ± 5% relative to the selenium content.     

Modeling calcium and water intake in threshed corn grain during thermo-alkaline treatment

A mathematical model describing simultaneous solvent diffusion and gelatinization of starch was used to explain the water and calcium absorption in threshed corn grains during the thermo-alkaline treatment. A computer-aided nonlinear optimization technique was used to find the effective diffusion coefficients and the reaction rate constants of water and calcium in threshed corn grains at boiling temperature (92.5 ± 0.3 °C). The mathematical model shows good correlation between measured and predicted values of water and calcium intake. It is concluded that the cooking process is limited by the reaction of starch components with water and calcium. The effective diffusion coefficient for water varied between 1.18 × 10⁻¹⁰ and 1.45 × 10⁻¹⁰ m²/s and for calcium between 8.55 × 10⁻¹⁰and 16.77 × 10⁻¹⁰ m²/s. The diffusion of water and calcium in threshed corn was produced with a reaction rate constants in the range of 6.83 × 10⁻⁴ to 10.4 × 10⁻⁴ s⁻¹ for water and 2.7 × 10⁻⁵–7.6 × 10⁻⁵ s⁻¹ for calcium. According to these effective diffusion coefficient values the diffusive process seems to be slower for water than for calcium. However, the reaction rate constant values are approximately 10 times higher for water than for calcium which may indicate that a higher amount of solvent was linked in the water diffusion process due to the gelatinization. Low concentration of Ca(OH)₂ such as 0.10% did not significantly affect the water diffusion of threshed corn during the cooking process.     

Evaluation of the influence of arsenical livestock drinking waters on total arsenic levels in cow’s raw milk from Argentinean dairy farms

The concentrations of total arsenic in cow’s raw milk and in the livestock drinking water were determined and compared, in order to establish the influence of natural arsenic levels in groundwaters on the final presence of arsenic in milk production of the most important dairy region in Argentina. A dry ashing procedure was used for the mineralisation of the milk samples. The total arsenic concentrations were determined by flow injection hydride generation atomic absorption spectrometry (FI-HGAAS). The mineralised milk samples and well water samples were pre-reduced with concentrated HCl and KI–C₆H₈O₆ solutions. A volume of 500 μl of each solution of pre-treated sample was transported by a HCl 1.2 mol l⁻¹ carrier solution at a flow rate of 11 ml min⁻¹ and merged with a reducing NaBH₄ 0.2% (m/v) solution which flowed at 5.5 ml min⁻¹. The hydride generated in a reaction coil was transported to the detector with a N₂ flow of 100 ml min⁻¹. The recovery values of added concentrations at levels of 2.5 μg l⁻¹ and 5.0 μg l⁻¹ of arsenic in milk were 103 ± 8% and 102 ± 6% for n = 3, respectively. The accuracy of the method for the determination of total arsenic in water was checked by analysis of a certified sample NIST 1643d. Detection limits were 0.7 μg l⁻¹ and 0.6 μg l⁻¹ for milk and well water, respectively. The results showed a low biological transference level of arsenic to the cow milk from the drinking water ingestion.     

Polymer films releasing nisin and/or natamycin from polyvinyldichloride lacquer coating: Nisin and natamycin migration,efficiency in cheese packaging

Polyethylene films coated by commercially available polyvinyldichloride (PVdC) as well as nitrocellulose (NC) lacquer with addition of natamycin preparation Delvocid® (16.7% w/w of natamycin in lacquer) were studied at 6 and 23 °C to determine the preservative migration into distilled water. The films released natamycin at maximal level 2.34 ± 0.32 mg/dm². The diffusion coefficient of 0.79 × 10⁻¹⁰ ± 0.29 × 10⁻¹⁰ cm²/s and 1.03 × 10⁻¹⁰ ± 0.17 × 10⁻¹⁰ cm²/s was determined for natamycin transport in PVdC lacquer layer at 6 and 23 °C, respectively. For nitrocellulose lacquer the diffusion coefficient of 0.89 × 10⁻¹⁰ ± 0.16 × 10⁻¹⁰ cm²/s was found at 23 °C. The coextruded polyamide/polyethylene film coated with the PVdC lacquer containing both nisin (16.7% w/w of preparation Nisaplin®) and natamycin (see above) provided inhibitory effect against selected indicator microorganisms (Penicillium expansum, Fusarium culmorum, Lactobacillus helveticus, Listeria ivanovií). This film was unsuitable for the packaging of the surface ripened cheese Olomoucké tvar??ky. On the other hand, it was able to prevent the growth of spoilage microorganisms on the surface of the packaged soft cheese Bla?ácké zlato.     

Direct determination of copper,lead and cadmium in aniseed spirits by electrothermal atomic absorption spectrometry

Direct determination of copper, lead and cadmium by electrothermal atomic absorption spectrometry in aniseed spirits was proposed. The methods were validated by studying quality parameters such as trueness, precision, linearity and sensitivity. Recoveries ranging between 96% and 104% were obtained from spiked samples at several concentration levels. Repeatability was less than 5% and intermediate precision was less than 8%. The procedure is fast and shows limits of detection of 0.6, 0.7 and 0.04 μg l⁻¹ for Cu, Pb and Cd, respectively. Samples were just diluted in a water/ethanol/nitric acid mixture. Cu was present at higher concentrations, with values in the range 6–473 μg l⁻¹. Minor levels of Pb and Cd were present with concentrations of less than 6 and 1.4 μg l⁻¹, respectively.