Effect of gamma-irradiation on flavour 5′-nucleotides,tyrosine, and phenylalanine in mushrooms (Agaricus bisporus)

The impact of gamma-irradiation on 5′-nucleotides and on the free amino acids tyrosine and phenylalanine in fresh mushrooms was studied. After irradiation the samples were freeze-dried to avoid enzyme induced chemical changes. Three 5′-nucleotides could be detected using HPLC–UV and LC–ESI-MS: adenosine 5′-monophosphate (AMP), guanosine 5′-monophosphate (GMP) and guanosine 5′-diphosphate (GDP). Irradiation significantly reduced (p = 0.05) the GDP concentration (22%). AMP showed a marked reduction (46%) only at 5 kGy. GMP, tyrosine, and phenylalanine were not affected by gamma-irradiation.     

Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid–liquid microextraction followed by gas chromatographic analysis

A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid–liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC–FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC–PCI–MS). Method was found to be linear over the range of 0.1–10 μg mL⁻¹ with square of correlation coefficient (R²) in the range of 0.9913–0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029–0.102 μg mL⁻¹ and 0.095–0.336 μg mL⁻¹ with a signal to noise ratio of 3:1 and 10:1, respectively.     

Development of polyclonal antibody-based indirect competitive enzyme-linked immunosorbent assay for sodium saccharin residue in food samples

A sensitive and specific polyclonal antibody (PcAb)-based indirect competitive enzyme-linked immunosorbent assay (icELISA) for sodium saccharin is described. 6-Amino saccharin was coupled to carrier protein for artificial antigen by diazotisation. New Zealand white rabbits were immunised to obtain anti-sodium saccharin PcAb and then icELISA was developed. The assay showed high sensitivity and specificity to sodium saccharin, with the 50% inhibition value (IC₅₀) of 0.243 μg mL⁻¹, workable range (IC₃₀–IC₇₀) of 0.050–12.8 μg mL⁻¹ and limit of detection (LOD, IC₂₀) of 0.021 μg mL⁻¹. The average recoveries of sodium saccharin in spiked food samples were estimated ranging from 70.7% to 98.8%. A statistically significant correlation of results was obtained between this new ELISA and previously established HPLC approaches with the food-relevant sodium saccharin concentration range 0–320 μg mL⁻¹ (R² = 0.9887–0.9975). These results indicated that the established ELISA was a potential and useful analytical tool for rapid determination of sodium saccharin residue in food samples.     

Non-volatile taste components of various broth cubes

Commercial soup bases, in the form of broth cubes available in the market, include chicken, mushroom, pork and seafood broth cubes. The non-volatile taste components of four broth cubes were studied. Equivalent umami concentration (EUC) values of these broth cubes were evaluated and compared with their sensory results from hedonic tests. Only two soluble sugars, lactose and sucrose, were found. Contents of total free amino acids and monosodium glutamate (MSG)-like components ranged from 0.51 to 1.04 mg g⁻¹ and 0.48 to 0.56 mg g⁻¹, respectively. Contents of 5′-nucleotides and flavour 5′-nucleotides ranged from 2.67 to 3.66 mg g⁻¹ and 2.58 to 3.33 mg g⁻¹, respectively. EUC values were low and the umami intensities of one gramme of four soup bases were equivalent to those given by 0.14–0.32 g MSG. Mushroom and pork soups were more preferred, whereas seafood soup was less preferred. Correlations of EUC values with sensory scores were established for chicken, pork and seafood soups.     

Rapid determination of formaldehyde and sulfur dioxide in food products and Chinese herbals

Simple, sensitive and rapid methods for the determination of formaldehyde and sulfur dioxide were developed. The formaldehyde determination is based on the reaction between formaldehyde and acetylacetone solution, producing yellow 3,5-diacetyl-l-1,4-dihydrolutidine. Sulfur dioxide was detected as the deoxidize of sulfurous acid by zinc in acidic medium, which produces sulfureted hydrogen that make lead acetate paper blackening due to lead sulfide formation. The detection limits were 0.8 μg mL⁻¹ and 6.0 μg mL⁻¹ for formaldehyde and sulfur dioxide, respectively. The linear range were 0.8–20.0 μg mL⁻¹ for formaldehyde and 6.0–100.0 μg mL⁻¹ for sulfur dioxide determination. The main advantages of the new analytical procedure are the low background level, high selectivity, and very little sample preparation for on-site analysis of formaldehyde and sulfur dioxide in food or Chinese herbal samples with reference color card for qualitative or semi-quantitative determination. The results from these methods correlated well with those obtained from the standard methods.     

Determination of melamine by flow injection analysis based on chemiluminescence system

In this paper, based upon the phenomenon that melamine can obviously enhance the CL signal of the luminol–H₂O₂ system in basic medium, a simple, rapid and sensitive flow injection chemiluminescence (FI-CL) method for the determination of melamine has been developed. Under the optimum conditions, the linear range for the determination of melamine was 0.2–80 μg mL⁻¹ with a detection limit of 0.12 μg mL⁻¹ calculated as proposed by IUPAC and a relative standard deviation of 3.26% for 11 solutions of 10 μg mL⁻¹ melamine on the same day. The proposed method was satisfactorily applied to determine melamine in milk-based products and satisfactory results were obtained without interferences from the sample matrix. Moreover, one assay produce takes only 25 s and the minimum sampling rate is about 120 samples h⁻¹, which indicated that the FI-CL method was suitable for high throughput and real-time melamine analysis.     

Flow injection analysis of total curcuminoids in turmeric and total antioxidant capacity using 2,2′-diphenyl-1-picrylhydrazyl assay

A simple flow injection analysis procedure is proposed for the determination of curcuminoids content in turmeric extracts. The method is based on the formation of a coloured complex between 4-aminoantipyrine and curcuminoids, in the presence of an oxidising reagent such as potassium hexacyanoferrate (III) in alkaline media. Conditions selected as a result of these trials were implemented in a flow injection analytical system in which the influence of injection volume, flow rate, reagent concentration and mixing coil length, was evaluated. Under the optimum conditions the total amount of curcuminoids could be determined within a concentration range of 5–50 μg mL⁻¹ which can be expressed by the regression equation y = 0.003x − 0.0053 (r² = 0.9997). The limits of detection and quantitation were found to be 0.6 μg mL⁻¹ and 1.8 μg mL⁻¹, respectively. The reproducibility of analytical readings was indicative of standard deviations <2%. The sample was extracted and analysed by using the proposed method. The percentage recoveries were found to be 94.3–108.0. The proposed system was applied to the determination of curcuminoids content in turmeric. The total curcuminoid contents in turmeric extract were found to be 0.9–4.3% (w/w). The development method is simple, economic, rapid and especially suitable for quality control in pharmaceutical plants.     

Spectrophotometric determination of melamine in milk by rank annihilation factor analysis based on pH gradual change-UV spectral data

A new spectrophotometric method has been developed in this paper to determine melamine in milk by applying rank annihilation factor analysis (RAFA) based on pH gradual change-UV spectral data (pH-spectra). In the proposed method, the spectra of the sample solutions at different pH data points were recorded and the pH-spectra bilinear data matrix was generated. Based on these data, the RAFA was then applied to calculate the concentration of melamine in milk. The experiments have been conducted and the results were satisfactory. Under the optimised conditions, linearity of the proposed method was in the range of 0.04–4.0 μg mL⁻¹ for calibration samples, and 0.04–3.5 μg mL⁻¹ for the mixed solutions of melamine with the background milk components. The detection limit (DL) was 12 ng mL⁻¹. The relative predictive error (RPEs) and root mean square error of prediction (RMSEP) of applying RAFA were 0.91% and 0.0151, respectively.     

A novel quantum dot-based fluoroimmunoassay method for detection of Enrofloxacin residue in chicken muscle tissue

A rapid indirect competitive fluorescence-linked immunosorbent assay (cFLISA) based on quantum dots (QDs) as the fluorescent marker has been developed for the detection of Enrofloxacin (ENR) in chicken muscle tissue. The end-point fluorescent detection system was carried out using QDs conjugated with goat anti-mouse secondary antibody. The cFLISA method allowed for ENR determination in a liner working range of 1–100 ng mL⁻¹ with the 50% inhibition value (IC₅₀) of 8.3 ng mL⁻¹ and the limit of detection (LOD) of 2.5 ng mL⁻¹. The recoveries for chicken muscle samples spiked with ENR at levels of 50–200 μg kg⁻¹ ranged from 81% to 94% with coefficients of variation (CV) of 10–13%. In real chicken tissue sample analysis, the results of cFLISA were similar to those obtained from an indirect competitive enzyme-linked immunosorbent assay (cELISA) to a high performance liquid chromatography method (HPLC), which indicated that cFLISA is suitable as screening method for the monitoring of veterinary drug residues.     

Rapid quantitation of curcumin in turmeric via NMR and LC–tandem mass spectrometry

A rapid, sensitive and accurate ¹H NMR method has been developed for the quantitation of curcumin isolated from Curcuma longa rhizome (turmeric) extract, the results of which were compared with a validated LC–MS/MS method. The relative standard deviations of the methods were found to be 2.49% and 3.48% for the ¹H NMR and LC–MS/MS methods, respectively. The correlation coefficients were 0.998 for ¹H NMR and 0.995 for LC–MS/MS assay in the calibration range. The recoveries at 5 mg mL⁻¹ and 50 μg mL⁻¹ concentrations averaged to 99–101% for both techniques, respectively. The uncertainty of the measurement of curcumin via ¹H NMR spectroscopy was determined to be 5.80% while in LC–ESI-MS/MS method was 7.38%.     

Determination of total phenols in tea infusions,tomato and apple juice by terbium sensitized fluorescence method as an alternative approach to the Folin–Ciocalteu spectrophotometric method

A fast screening of total phenols in tea infusions, tomato and apple juice samples using terbium sensitized fluorescence is described. The proposed method is based on the fluorescence sensitization of terbium (Tb³⁺) by complexation with flavonols (quercein as a reference standard) (at pH 7.0), which fluoresces intensely with an emission maximum at 545 nm when excited at 310 nm. Quercetin and terbium cations (at pH 7.0) form a stable complex and the resulted emission at 545 nm can be used for the determination of the total phenols concentration expressed in terms of “quercetin equivalent”. Based on the obtained results, a sensitive, simple and rapid spectrofluorimetric method was developed for the determination of total phenols. In the optimum conditions, the calibration graph was linear from 0.01 to 2 μg mL⁻¹, with the limit of detection of 0.002 μg mL⁻¹. The relative standard deviation values were in the range of 0.75–2.3%. The total concentrations of quercetin equivalent in five tested samples were found in the range of 6.6–27.9 μg mL⁻¹ and the results compare favorably with those obtained by spectrophotometric method (r = 0.999).     

Non-volatile taste active compounds in the meat of Chinese mitten crab (Eriocheir sinensis)

The non-volatile taste active compounds, including soluble sugars, succinic acid, free amino acids and flavour 5′-nucleotides in the meat of Chinese mitten crab (Eriocheir sinensis) were analyzed, and their taste impacts were evaluated by taste active values (TAVs) and equivalent umami concentration (EUC) methods. The total free amino acid content of crab meat was 20.9 mg/g. Arginine, glycine and alanine were the major free amino acids, accounting for more than 70% of the total free amino acids. 5′-Adenosine monophosphate (AMP) was the main flavour 5′-nucleotide (75.3 mg/100 g), followed by 5′-inosine monophosphate (IMP) (34.4 mg/100 g) and 5′-guanosine monophosphate (GMP) (2.3 mg/100 g). Arginine, glycine, alanine, glutamic acid, IMP and AMP were of high TAV (greater than one), and they had strong taste impacts on the crab meat flavour. Glycine and alanine contributed to the major sweet taste, while glutamic acid, IMP and AMP contributed to the strong umami taste. As the TAVs of soluble sugar, succinic acid and bitter free amino acids were lower than one, thus those compounds are likely to have insignificant impact on the taste of the crab meat. The EUC was 4.2 g MSG/100 g crab meat, which meant that the umami taste of the crab meat was very intense.     

Isolation and properties of 5′-nucleotidase isolated from jumbo squid (Dosidicus gigas) mantle muscle from the Gulf of California,Mexico

The enzyme 5′-nucleotidase of jumbo squid (Dosidicus gigas) mantle was purified and its SDS–PAGE showed a single band of 33 kDa, whereas a protein with a molecular mass of 107 kDa was detected by gel filtration suggesting a homotrimeric nature of this enzyme. Subunits of the named enzyme were not linked by covalent bonds. Isoelectric focusing of this enzyme showed a pI of 3.6–3.8 and presented a hyperbolic kinetics with V_max of 1.16 μM/min/mg of protein, K_m of 1.49 mM, K_cat of 3.48 μM of P_ι s⁻¹ and K_cat/K_m relation of 356.52 ((mol/L)⁻¹ s⁻¹). Purified enzyme preferred AMP as substrate (by 6.7-folds) than IMP, showing a K_m of 6.34 mM, V_max of 0.19 μM/min/mg of protein a K_cat of 0.3388 mol of P_ι s⁻¹ and K_cat/K_m relation of 53.44 ((mol/L)⁻¹ s⁻¹). The low K_m in relation to purified AMP deaminase of the same organism suggested a high contribution of 5′-nucleotidase in AMP degradation in jumbo squid mantle.     

Trace element levels in honeys from different regions of Turkey

A survey of 25 honey samples from different botanical origin, collected all over the Turkey was conducted to assess their trace element contents. The aim of this study was to determine the levels of cadmium (Cd), lead (Pb), iron (Fe), manganese (Mn), copper (Cu), nickel (Ni), chromium (Cr), zinc (Zn), aluminium (Al) and selenium (Se) in honey samples from different regions of Turkey. Trace element contents were determined by a flame and graphite furnace atomic absorption spectrometry technique after dry-ashing, microwave digestion and wet-digestion. The accuracy of the method was corrected by the standard reference material, NIST-SRM 1515 Apple leaves. The contents of trace elements in honey samples were in the range of 0.23–2.41 μg g⁻¹, 0.32–4.56 μg g⁻¹, 1.1–12.7 μg g⁻¹, 1.8–10.2 μg g⁻¹, 8.4–105.8 μg kg⁻¹, 2.6–29.9 μg kg⁻¹, 2.4–37.9 μg kg⁻¹, 0.9–17.9 μg kg⁻¹, 83–325 μg kg⁻¹ and 38–113 μg kg⁻¹ for Cu, Mn, Zn, Fe, Pb, Ni, Cr, Cd, Al and Se, respectively. Iron was the most abundant element while cadmium was the lowest element in the Turkish honeys surveyed. The results showed that trace element concentrations in the honeys from different regions were generally correlated with the degree of trace element contamination of the environment.     

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.     

Pharmacokinetics and residues of tetracycline in crucian carp muscle using capillary electrophoresis on-line coupled with electrochemiluminescence detection

A novel and sensitive determination for tetracycline (TC) in crucian carp muscle was developed by using capillary electrophoresis coupled with electrochemiluminescence (ECL) detection. The conditions affected separation and detection were examined in detail. The linearity range of TC concentration was from 0.005 to 10 μg mL⁻¹ with a correlation coefficient of 0.9992. The detection limit of TC (S/N = 3) was 1.8 ng mL⁻¹. The relative standard deviations of the ECL intensity and the migration time for eleven consecutive injections of 1.0 μg mL⁻¹ TC were 1.6% and 0.8%, respectively. The recovery of TC was 97.8% (n = 5). After administration of 75 mg kg⁻¹ TC, the maximum concentration and peak time of TC in crucian carp muscle were 7.33 mg kg⁻¹ and 8 h, respectively. After administration of TC, TC concentration demonstrated trivial variation in the period from 48 to 96 h.     

Residue levels of food-grade antioxidants in postharvest treated in-pod peanuts during five months of storage

In order to investigate residue levels of butylated hydroxyanisole (BHA), propyl paraben (PP) and butylated hydroxytoluene (BHT) during storage, eight-hundred kilograms of bulk peanuts were treated with the following antioxidant emulsions: BHA (1802 μg g⁻¹), BHA–PP (1802 μg g⁻¹ + 1802 μg g⁻¹) M1 and BHA–PP–BHT mixtures (1802 μg g⁻¹ + 901 μg g⁻¹ + 2204 μg g⁻¹) M2 and (1802 μg g⁻¹ + 1802 μg g⁻¹ + 2204 μg g⁻¹) M3. Residues were determined in peanut pod and seed tissues at 1-month intervals during the storage. While the reduction levels of BHA and PP in pods at the end of the storage period ranged from 66% to 76%, BHT levels were decreased extensively (86%). Twenty-four hours after peanuts were treated, antioxidant emulsions effectively seeped into the seeds and low levels of these chemicals were detected during the assay. Residues of PP in seeds were lower (62%) than the other antioxidants. Although the doses used were higher than those approved for food-grade antioxidants in stored peanuts, the residue levels in seeds (32.8–0.02 μg g⁻¹) did not exceed the maximum residue limits during the storage period.     

Simultaneous voltammetric analysis of tetracycline antibiotics in foods

The new simple, cost effective and well performing differential pulse stripping voltammetry method for the simultaneous determination of antibiotics – oxytetracycline, tetracycline and chlorotetracycline was researched and developed. It depends on the reduction of these compounds at a hanging mercury drop electrode. The samples were extracted from (i) spiked animal feed, and (ii) fresh fish muscle dosed with the drugs. The voltammograms from the drug mixture produced complex, overlapping profiles, and chemometrics methods were applied for calibration modelling. The analytical linear ranges were within 0.02–0.18 μg mL⁻¹ and the corresponding LODs were 3–5 μg L⁻¹ for the three analytes. These values compare well with those from the HPLC and fluorescence methods in the literature. The % relative prediction errors from the verification trials were between 4% and 9% with % Recoveries being 103–107. Also, the % Recoveries of the antibiotics from animal feeds as measured by the new method were comparable with those from the HPLC analysis (85%), i.e. the method is highly competitive, especially as a screening approach.     

Microwave-assisted extraction and determination of cyanuric acid residue in infant formula samples by liquid chromatography–tandem mass spectrometry

In the present work, microwave-assisted extraction method in combining with liquid chromatography–tandem mass spectrometry (LC–MS/MS) was proposed for the determination of cyanuric acid (CYA) in infant formula samples. The separation was performed on a MERCK ZIC HILIC column (150 × 2.1 mm i.d., 5 μm) with gradient elution of 20 mM ammonium acetate solution – acetonitrile. The method could respond linearly with cyanuric acid at concentrations from 1.0 to 50 ng mL⁻¹ with a quantification limit of 0.25 mg kg⁻¹. The intra- and inter-day precision was less than 4% and the recovery of the assay was in the range of 86.7–93.1%. In the analysis of practical spiked infant formula samples, the new method yielded satisfactory results. Due to its simplicity and accuracy the straightforward method is particularly suitable for routine cyanuric acid detection.     

Effect of modifiers for As,Cu and Pb determinations in sugar-cane spirits by GF AAS

Palladium plus magnesium nitrates with and without Ir, Ru and W were evaluated for the simultaneous determination of As, Cu and Pb in cachaça by graphite furnace atomic absorption spectrometry. For 20 μL of sample, 5 μL Pd(NO₃)₂ and 3 μL Mg(NO₃)₂ dispensed together onto the Ir-coated platform of the THGA, analytical curves in the 0–30.0 μg L⁻¹ As, 0–1.50 mg L⁻¹ Cu and 0–60.0 μg L⁻¹ Pb were built up and typical linear correlation coefficients were always better than 0.999. The limit of detection was 1.30 μg L⁻¹ As, 140 μg L⁻¹ Cu and 0.90 μg L⁻¹ Pb. As, Cu and Pb contents in 10 cachaça samples agreed with those obtained by ICP-MS. Recoveries of spiked samples varied from 96% to 106% (As), 97% to 112% (Cu) and 92% to 108% (Pb). The relative standard deviation (n = 12) was typically 2.7%, 3.3% and 1.9%.