Comparison of graphite furnace and hydride generation atomic absorption spectrometry for the determination of selenium status in chicken meat

Four different procedures for the determination of selenium in chicken meat by atomic absorption spectrometry were investigated. They consisted on conventional ambient pressure acid digestion carried out before and after sample drying, associated or not with fat extraction. For all procedures muscle and skin were analyzed separately. Drying was carried out in a conventional oven at 65 °C for 24 h. For fat extraction different solvents and solvent mixtures were investigated considering both extraction yield and sample adequacy for further AAS measurement. Acid digestions were carried out with mixtures of HNO₃ and HClO₄. After digestion, selenium was measured either by Hydride Generation (HGAAS) or by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). For the reduction of Se(VI) prior to the HGAAS determination, 8% (w/v) NaBr, 6 mol/l HCl (both with and without sulfamic acid), as well as UV radiation were investigated. Tests with spiked samples have shown that either UV radiation (pH 8) or NaBr/sulfamic acid presented good recoveries. In this way the HGAAS determination of selenium in tissue was carried out without interference whereas for the fatty fraction the results were satisfactory only if GFAAS was used. The results showed that drying the sample and extracting the fat prior to digestion is advantageous once the amount of acid necessary can be significantly reduced. The precision, expressed as relative standard deviation, was about 6.5% and 0.8% for GFAAS and HGAAS measurements, respectively. The limits of detection for HGAAS and GFAAS, based on three times the standard deviation of the blanks were 1 μg/l and 0.6 μg/l, respectively. The results have shown that in chicken meat 59% of the selenium is found in the muscle tissue while the skin responds for 41%.     

Accumulation of arsenic in different fresh water fish species – potential contribution to high arsenic intakes

The aim of the study was to evaluate total arsenic (As) in five tissues (gills, mouthpiece, intestine, liver and muscles) of 10 fish species caught from As contaminated Manchar Lake (26°3′N: 67°6′E) Sindh Pakistan during 2006–2007. The total As concentration was determined by hydride generation atomic absorption spectrometry (HG-AAS), prior to microwave assisted acid digestion. The certified reference material DORM-2 (dogfish muscle) was used to check the quality control of the technique. The good agreement with the certified value at 95% confidence limit confirmed the validity of As determination method. The limit of detection (LOD) and limit of quantitation (LOQ) of As were 0.034 and 0.11 μg/g, respectively.     

Determination of trace element contents of baby foods from Turkey

The levels of trace elements in different types of baby foods consumed in Turkey were determined by flame and graphite furnace atomic absorption spectrometry. Dry, wet and microwave digestion procedures were compared and the microwave digestion method was found to be the best. The accuracy of the method was ensured by using a standard reference material (NIST-SRM 8418 Wheat Gluten). The levels of elements in analyzed samples were found to be under legal limits. The range of the investigated elements were 0.52–4.38 μg/g, 0.22–7.20 μg/g, 1.02–67.5 μg/g, 0.92–37.2 μg/g, 0.12–0.32 μg/g, 2.02–68.8 μg/kg, 10.7–66.8 μg/kg, 0.05–10.3 μg/g, 2.67–25.4 μg/kg for Cu, Mn, Fe, Zn, Se, Cr, Al, Ni and Co, respectively.     

Development of a highly sensitive and specific monoclonal antibody-based enzyme-linked immunosorbent assay for determination of doxycycline in chicken muscle,liver and egg

A modified indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) method was developed using a highly sensitive and specific monoclonal antibody (McAb) to determine doxycycline (DC) residues in chicken tissues and egg. The McAb against DC was produced by hybridoma technique and a modified ic-ELISA was characterised in terms of sensitivity, specificity, precision and accuracy. At optimal experimental conditions, the standard curve was constructed at concentrations ranged from 0.01 to 100 ng/ml. The IC₅₀ value was 1.32 ± 0.18 ng/ml. The limit of detection was 0.14 ± 0.02 ng/g. The recoveries of DC from spiked chicken liver, muscle, and egg at levels of 50–600 ng/g were 84.6–85.5%, 88.2–89.1%, and 84.4–89.3%, respectively. The coefficient variations (CVs) were 5.1–9.3%, 3.7–11.3%, and 4.7–9.8%, respectively. Linear regression analysis showed good correlation, with r² values 0.9909 for chicken liver and 0.9916 for chicken muscle.     

Fumonisin level in corn-based food and feed from Linxian County,a high-risk area for esophageal cancer in china

The level of mycotoxin fumonisins in corn-based food and feed collected from Linxian County, a high-risk area for esophageal cancer in China, has been analyzed using high-performance liquid chromatographic coupled with evaporative laser scattering detector (HPLC-ELSD). A total of 104 corn kernel samples were obtained from local households, granaries, wholesale markets (central markets), and retail markets (stores and supermarkets). Fumonisin B₁ (FB₁) was detected in the samples from households, granaries, central markets, and stores, with a positive rate of 61.5%, 50%, 33.3%, and 17%, respectively. No fumonisin was detected in samples from the supermarket. The highest FB₁ levels (0.30–3.20 μg/g; mean, 1.42 μg/g) were found in samples from the granary, followed by household (0.25–1.80 μg/g; mean, 0.73 μg/g), central market (0.25–1.10 μg/g; mean, 0.51 μg/g), and store (0.22–0.34 μg/g; mean, 0.28 μg/g). Among the 80 corn kernel samples collected from local households, 18 of 24 (75.0%) moldy samples contained high levels of FB₁ (0.28–3.30 μg/g; mean, 1.58 μg/g), and 20 of 56 (35.7%) apparently healthy samples contained low levels of FB₁ (0.21–0.82 μg/g; mean, 0.46 μg/g). As the central market plays an important role in trade of corn-based food and feed in China, a total of 115 corn-based food and feed samples were collected from the local central market. The highest FB₁ levels (0.30–3.13 μg/g; mean, 1.50 μg/g) were found in feed, followed by unprocessed food (0.31–0.63 μg/g; mean, 0.47 μg/g) and processed food (0.21–0.28 μg/g; mean, 0.25 μg/g). The positive incidence of FB₁ in feed, unprocessed, and processed food were 53.6%, 33.3% and 17.9%, respectively. In conclusion, the results showed that corn-based food and feed from Linxian County contained low level of FB₁ (<2 μg/g) in general, but efforts should be made to control the fumonisin contamination in corn kernels stored in granaries and households.     

Effect of refining processes on antioxidant capacity,total contents of phenolics and carotenoids in palm oils

Antioxidant capacity (AC), total phenolic content (TPC) and total carotenoid content (TCC) in palm oils at various stages of the refining process from two technological modes were determined. The obtained mean FRAP and DPPH values for the methanolic extracts of palm oils from mode 1 (19.5–102.8 μmol TE/100 g and 18.8–103.0 μmol TE/100 g) were lower than for oils from mode 2 (25.6–134.8 μmol TE/100 g and 25.4–135.4 μmol TE/100 g). The total phenolics (4.1–12.4 mg GA/100 g) and carotenoids (0.18–45.8 mg/100 g) in the studied oils were correlated with their antioxidant capacities determined by FRAP and DPPH methods (r = 0.6623–0.9878). During the refining process, for both technological modes resulted in a loss of AC by 80%, TPC by 26–55% and TCC by 99%. The bleaching step caused the highest losses of AC as determined by FRAP 41% and 46%, DPPH by 43% and 48%, while TPC loss was 45% and 23% and loss of carotenoids was 49% and 56%, in mode 1 and mode 2, respectively.     

Mercury and its bioconcentration factors in Brown Birch Scaber Stalk (Leccinum scabrum) from various sites in Poland

The total mercury contents were determined in the carpophores of Brown Birch Scaber Stalk (Leccinum scabrum) and topsoil (0–10 cm) collected from 12 spatially distant sites across Poland. Mercury was measured by cold-vapour atomic absorption spectroscopy (CV-AAS) after nitric acid (mushrooms) or aqua regia (soil) digestion of the samples. The caps, depending on the site, had total mercury concentrations from 0.38 ± 0.23 to 1.2 ± 0.4 μg/g dm (median 0.36–1.2 μg/g dm), and stalks from 0.17 ± 0.08 to 0.72 ± 0.20 μg/g dm (median 0.17–0.72 μg/g dm). Overall-mean mercury contents for 240 caps and stalks were 0.63 ± 0.38 (0.072–2.0 μg/g dm) and 0.32 ± 0.20 (0.028–1.2 μg/g dm), respectively. The total mercury content in top soil layer (0–10 cm) at 12 sites, after hot aqua regia extraction, averaged 0.026 ± 0.010–0.066 ± 0.018 μg/g dm. The BCF values of total mercury in caps of Brown Birch Scaber Stalk from the particular sites ranged from 14 ± 5 to 20 ± 4 (total mean was 16 ± 5, and median 18), in stalks from 6.0 ± 4.0 to 11 ± 1 (total mean was 8.3 ± 3.1, and median 8.1). In human feeding, wild mushrooms are usually only a small part of the total diet, so consumption of Brown Birch Scaber Stalk collected from the background sites in Poland, or elsewhere in Europe, as regards mercury content, could be considered safe.     

Determination of trace metals in canned fish marketed in Turkey

The levels of trace metals of canned fish samples collected from markets in Turkey were determined by flame and graphite furnace atomic absorption spectrometry after microwave digestion. The accuracy of the method was corrected by standard reference material (NRCC-DORM-2 Dogfish Muscle). The contents of investigated trace metals in canned fish samples were found to be in the range 1.10–2.50 μg/g for copper, 7.57–34.4 μg/g for zinc, 0.90–2.50 μg/g for manganese, 10.2–30.3 μg/g for iron, 0.96–3.64 μg/g for selenium, 0.45–1.50 μg/g for aluminium, 0.97–1.70 μg/g for chromium, 0.42–0.85 μg/g for nickel, 0.09–0.40 μg/g for lead and 0.06–0.25 μg/g for cadmium. The results were compared with the literature values.     

Trace metal content in nine species of fish from the Black and Aegean Seas,Turkey

Trace metal content of nine fish species harvested from the Black and Aegean Seas were determined by microwave digestion and atomic absorption spectroscopy (MD–AAS). Verification of the MD–AAS method was demonstrated by analysis of standard reference material (NRCC-DORM-2 dogfish muscle). Trace metal content in fish samples were 0.73–1.83 μg/g for copper, 0.45–0.90 μg/g for cadmium, 0.33–0.93 μg/g for lead, 35.4–106 μg/g for zinc, 1.28–7.40 μg/g for manganese, 68.6–163 μg/g for iron, 0.95–1.98 μg/g for chromium, and 1.92–5.68 μg/g for nickel. The levels of lead and cadmium in fish samples were higher than the recommended legal limits for human consumption.     

Effect of canned tuna fish processing steps on lead and cadmium contents of Iranian tuna fish

The contents of Pb and Cd in two species of Iranian tuna fish (yellowfin and skipjack), which were caught from the Persian Gulf and Oman Sea, and the effects of canning processing steps on their contents were assessed by electrothermal atomic absorption spectrometry. The results revealed that the levels of lead and cadmium throughout the processing steps in yellowfin were in range of 0.154 ± 0.019–0.441 ± 0.025 μg/g and 0.029 ± 0.002–0.084 ± 0.0005 μg/g, respectively. Pb and Cd concentrations from received fish to final product in skipjack were found to be in range of 0.072 ± 0.031–0.218 ± 0.031 μg/g and 0.016 ± 0.001–0.062 ± 0.002 μg/g, respectively. The limit of detection for lead and cadmium were 0.058 μg/g (11.6022 μg/l) and 0.0007 μg/g (0.1485 μg/l), respectively. Results from paired sample t-test analysis showed that defrosting, cooking, and sterilisation by autoclave would reduce the contents of lead and cadmium, considerably.     

Development of an HPLC–UV method for the simultaneous determination of tetracyclines in muscle and liver of porcine,chicken and bovine with accelerated solvent extraction

A simple and especially rapid method-using accelerated solvent extraction (ASE) and HPLC has been developed for the quantitative determination of oxytetracycline, tetracycline, chlortetracycline, minocycline, methacycline, demeclocycline and doxycycline in muscle and liver of porcine, chicken and bovine. Samples of muscle and liver were extracted with trichloracetic acid/acetonitrile using ASE instrument, parameters such as extraction temperature (40–80 °C) and pressure (45–85 bar) were investigated and the selected extraction (60 °C, 65 bar) was most effective. The limits of detection were lower than 10 μg/kg and limits of quantification no more than 15 μg/kg for all compounds in muscle and liver. The recoveries of tetracyclines spiked at levels of muscle 50–150 μg/kg, liver 150–450 μg/kg, averaged from 75.0% to 104.9% with the relative standard deviation values less than 10%. The method was applied to determine 30 real porcine livers. It is demonstrated that the new method is robust for detection and quantification of seven tetracycline residues in muscle and liver of porcine, chicken and bovine.     

Evaluation of trace element contents in canned foods marketed from Turkey

Trace element contents of 10 canned foods (mushroom, corn, pea, mixed vegetable, tomato, red mullet, stuffed grape leaves, pickle, bean, delicatessen) from Turkish markets were determined by flame and graphite furnace atomic absorption spectrometry after microwave digestion. The accuracy of the method was determined by use of a standard reference material (NIST SRM 1573a Tomato Leaves). The contents of investigated trace elements in canned foods were found to be in the range of 2.85–7.77 μg/g for copper, 8.46–21.9 μg/g for zinc, 6.46–18.6 μg/g for manganese, 27.5–79.6 μg/g for iron, 0.05–0.35 μg/g for selenium, 0.93–3.17 μg/g for aluminium, 0.19–0.52 μg/g for chromium, 0.18–0.75 μg/g for nickel, and 0.20–1.10 μg/g for cobalt. The results found were compared with those reported by scientists from various countries.     

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.     

Development of an enzyme-linked immunoassay for the detection of gentamicin in swine tissues

We developed an enzyme-linked immunoassay that provides rapid and sensitive detection of gentamicin in swine tissues. Rabbit was immunized with gentamicin-BSA conjugate and antiserum was collected after the fifth immunization. After optimizing the concentration of immunoreagents, competitive indirect ELISA (ciELISA) gave an IC₅₀ value of 0.98 ng/ml, while competitive direct ELISA (cdELISA) exhibited lower IC₅₀ value of 0.92 ng/ml, thus cdELISA was further optimized under various pH values and ionic strengths of assay buffer, different coating methods and incubation time. The optimized ELISA can be completed within 45 min and it showed negligible cross-reactivity with other aminoglycosides. The recoveries of gentamicin from spiked swine tissues at levels of 25–200 μg/kg ranged from 64.7% to 101.2% with CVs of 4.5–12.1%, and the detection limits were 6.2 μg/kg in muscle, 3.6 μg/kg in liver and 2.7 μg/kg in kidney, respectively.     

Determination of inorganic arsenic species (As and As) in muscle tissues of fish species by electrothermal atomic absorption spectrometry (ETAAS)

Arsenic speciation was carried out in muscle tissues of freshwater fish species. Inorganic arsenic species (As³⁺and As⁵⁺) were extracted with chloroform, prior to microwave assisted digestion with concentrated HClO₄ and Fe₂(SO₄)₃. The extracted As³⁺ and As⁵⁺ were determined by electrothermal atomic absorption spectrometry (ETAAS). The accuracy of the technique was evaluated by using certified reference material DORM-2. The limit of detection of the method was 0.004 and 0.005 μg/g for As³⁺ and As⁵⁺, respectively. The mean relative standard deviation values (RSD) in real sample analysis were 1.90 and 3.92 for As³⁺ and As⁵⁺, respectively. The results demonstrated the suitability of the procedure for screening and quantification of As species in biological samples. The mean concentration of As³⁺ and As⁵⁺ in muscle tissues of studied fish species ranged from 1.19 to 2.05 and 0.17 to 0.46 μg/g, respectively. The contribution of the daily intake of inorganic As, based on the consumption of 250 g fresh fish muscles/body weight/day was found in the range of 1.21–1.91 μg/kg/day.     

Monitoring and risk assessment of pesticide residues in yuza fruits (Citrus junos Sieb. ex Tanaka) and yuza tea samples produced in Korea

The objective of this study was to establish an analytical method to measure pesticides used to cultivate yuza (Citrus junos Sieb. ex Tanaka) and to analyze pesticide residue levels of yuza and yuza tea samples. Risk assessments were also performed by calculating estimated daily intake (EDI) and acceptable daily intake (ADI). An excellent linear correlation was achieved with coefficient correlation values of 0.9750–0.9999. Percent recoveries were 80.4–109.9% for most pesticides with a <6.9% relative standard deviation (RSD). The limits of quantification for the method were 0.10–0.67 μg/ml. The RSD of intra-day and inter-day variability was <15.3%. Seven pesticides in yuza (n = 80) and yuza tea (n = 75) were analyzed with the optimized analytical method. Acequinocyl, spirodiclofen and carbendazim were detected in yuza samples in the concentration range of 0.07–0.15 μg/g, 0.11–1.89 μg/g, and 0.03–5.15 μg /g, respectively, whereas chlorpyrifos, prothiofos, phosalone, and deltamethrin were not detected in yuza or yuza tea. The concentrations of acequinocyl, spirodiclofen and carbendazim ranged from 0.18–1.05 μg/g, 0.13–0.29 μg/g, and 0.17–2.36 μg/g, respectively, in yuza tea samples. The percent ratios of EDI to ADI for acequinocyl, spirodiclofen, and carbendazim were 24.6%, 22.7%, and 58.5%, respectively.     

Fatty acids and cholesterol oxidation in salted and dried shrimp

The aim of this work was to evaluate the occurrence of cholesterol oxidation products and to analyze the lipidic profile in salted–dried shrimp. Fifty samples of salted–dried shrimp were evaluated, and the cholesterol oxides (7β-OH, 7α-OH, 7-Keto and 25-OH) were quantified by high-performance liquid chromatography. The cholesterol oxides: 7β-OH (34.63–72.56 μg/g), 7α-OH (5.02–12.12μg/g), 7-Keto (7.44–32.68 μg/g) and 25-OH (2.37–22.88 μg/g) were determined in all samples analyzed. Regarding to the total cholesterol content and the average thiobarbituric acid reactive substances (TBARS) content, the results ranged from 73.88 to 247.69 mg/100 g, and 0.02 to 1.30 mgMA/kg, respectively. The fatty acids profile was: 27.48% saturated, 43.90% monounsaturated and 28.61% polyunsaturated. The presence of cholesterol oxidation products and the values of TBARS indicate the degree of oxidation of this product, which was probably initiated by inadequate conditions of processing and storage.     

Determination of catechins in green tea infusions by reduced flow micellar electrokinetic chromatography

A sulfated-β-cyclodextrin (s-β-CD) modified reduced flow micellar electrokinetic chromatography (RF-MEKC) method was developed and validated for the determination of catechins in green tea. The optimal electrolyte consisted of 0.2% triethylamine, 50 mmol/L SDS and 0.8% s-β-CD (pH = 2.9), allowing baseline separation of five catechins in 4 min. The samples and standards were injected at 0.6 psi for 5 s under constant voltage of −30 kV. Sample preparation simply involved extraction of 2 g of tea with 200 mL water at 95 °C under constant stirring for 5 min. The method demonstrated excellent performance, with limits of detection (LOD) and quantification (LOQ) of 0.02–0.1 and 0.1–0.5 μg/mL, respectively, and recovery percentages of 94–101%. The method was applied to six samples of Brazilian green tea infusions. Epigallocatechin gallate (23.4–112.4 μg/mL) was the major component, followed by epigallocatechin (18.4–78.9 μg/mL), epicatechin gallate (5.6–29.6 μg/mL), epicatechin (4.6–14.5 μg/mL) and catechin (3.2–8.2 μg/mL).     

Anti-oxidative analysis,and identification and quantification of anthocyanin pigments in different coloured rice

Anthocyanin pigments in coloured rice cultivars were isolated and identified using high-performance liquid chromatography techniques. Two black rice cultivars (Asamurasaki, Okunomurasaki) contained three major anthocyanins: cyanidin-3-glucoside, peonidin-3-glucoside and malvidin. Chinakuromai (black) rice additionally contained a fourth anthocyanin, petunidin-3-glucoside. Four red rice cultivars contained only malvidin. The total anthocyanin content varied greatly among black rice cultivars (79.5–473.7 mg/100 g), but was lower in red rice (7.9–34.4 mg/100 g). Total phenolic content was similar between red (460.32–725.69 mg/100 g) and black (417.11–687.24 mg/100 g) rice. The oxygen radical absorbing capacity was ranked as follows: red (69.91–130.32 μmol Trolox/g) > black (55.49–64.85 μmol Trolox/g) > green (35.32 μmol Trolox/g) > white (21.81 μmol Trolox/g) rice. The antioxidant capacity resulted mainly from the seed capsule, not the endosperm. The anthocyanin pigments contributed little to the total antioxidant capacity of red (0.03–0.1%) and black (0.5–2.5%) rice cultivars. Hence, the antioxidant capacity is derived mainly from other phenolic compounds.     

Folate contents of some selected Fijian foods using tri-enzyme extraction method

Folic acid and total folate contents of 18 common foods in the Fijian diet were assayed. Foods were purchased from the central and eastern parts of Viti Levu in Fiji. Tri-enzyme treatment was performed to release bound folates using protease and α-amylase, with chicken pancreas as the conjugase. The highest total folate content was recorded for egg yolk (Gallus domesticus) at 256 μg/100 g, followed by long beans (Vigna sesquipedalis) which contained 130 μg/100 g of total folate (fresh weight basis). The local leafy vegetable called Bele (Abelmoschus manihot) and the Drumstick leaves (Moringa oleifera) available in Fiji also had high total folate contents, above 100 μg/100 g (fresh weight basis). For the 18 foods studied, the content of folic acid ranged from 3 to 189 μg/100 g and the total folate content was in the range of 3–256 μg/100 g, indicating a very wide range of folate content in the foods studied.