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1.
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.  相似文献   

2.
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.  相似文献   

3.
Trace element levels in honeys from different regions of Turkey   总被引:1,自引:0,他引:1  
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.  相似文献   

4.
A method based on matrix solid-phase dispersion (MSPD) was developed for the quantitative extraction of five organophosphorus (OPPs) pesticides from bovine samples. The determination was carried out by high performance liquid chromatography (HPLC) with diode array spectrophotometric UV detection. The MSPD extraction with octadecylsilyl (C18) sorbent combined with a silica gel clean-up and acetonitrile elution was optimised for chlorpyrifos, chlorfenvinphos, diazinon, fenitrothion, and parathion-methyl. The method was validated, yielding recovery values higher than 94%, except for chlorfenvinphos in liver (55%), and precision values, expressed as relative standard deviations (RSDs), which were less than or equal to 15% in liver and 11.5% in muscle at spiking levels of 0.25, 2.5 and 5 μg g−1. Linearity was studied from 0.5 to 15 μg g−1, and the limits of detection (LODs) were found to be lower than 0.1 μg g−1. This method was applied to the analysis of real samples with confirmative analyses performed using gas chromatography–mass spectrometry (GC–MS) in selected ion monitoring mode (SIM).  相似文献   

5.
A fast, simple and effective extraction method based on matrix solid phase dispersion (MSPD) was developed and validated for the simultaneous cleaning-up and quantitative extraction of illegal dyes (sudan I, sudan II, sudan III and sudan IV) from different sauces and condiments. Several parameters as sorbent, cleaning procedure to eliminate carothenoids and other interferences, and solvents for elution were evaluated to find the optimal MSPD conditions. The best results were obtained using a system containing washed sea sand and Florisil as sorbents and sodium sulphate as desiccant; hexane was used as defatted agent and acetonitrile as elution solvent. Quantitative analyses were performed by liquid chromatography (LC) with diode array detection (DAD). The chromatographic separation was performed on a Phenomenex Synergy Polar RP column with isocratic elution using methanol/acetonitrile/water 65/20/15, v/v/v, as the mobile phase at a flow rate of 1.0 mL min−1 and 30 °C of temperature. Under these conditions sudan I–IV recoveries were between 60% and 99% and relative standard deviations ranging from 2.0% to 10.0%. Limits of detection resulted five times lower than the values required by European regulations and were ranged between 0.05 and 0.09 μg g−1. The applicability of this MSPD–DAD method to determine illegal sudan dyes in sauce and condiment samples was demonstrated. This method has potential to be applied using a simple instrumentation present in most analytical laboratories.  相似文献   

6.
An optimal condition of supercritical fluid extraction (SFE) for isoflavone aglycones (daidzein and genistein) in soybean hypocotyls previously subjected to thermohydration at pH 5.0 and a temperature of 50 °C for 6, 12 and 18 h was developed. Different temperatures, pressures and cosolvents (methanol, ethanol, and acetonitrile) was tested and compared with solid–liquid extraction using aqueous methanol solution (80% v v−1) conducted in parallel for comparison. The extraction conditions were 50–70 °C, 176–380 bar, adding 0, 5, 10 mol% of cosolvents 80% in water as a modifier. The results from SC–CO2 showed that the cosolvent and pressure have significant effects in the extraction efficiency. It was found that the extraction conditions promoting the highest extraction of daidzein and genistein were at the temperature of 60 °C, pressure of 380 bar and both static and dynamic extraction of 15 min with the addition of 10% acetonitrile (80% v v−1). The maximum amounts of daidzein and genistein extracted by each method were solid–liquid extraction (70.07 mg 100 g−1) and carbon dioxide–acetonitrile (17.97 mg 100 g−1). The yield of daidzein and genistein achieved by a 30 min SC–CO2 extraction on soybean hypocotyls after 12 h soaking time was markedly improved by the addition of a modifier (acetonitrile) to the CO2 fluid. HPLC analysis of the obtained extracts revealed that extraction of isoflavone aglycones by SC–CO2 was 4.78 and 13.19 mg 100 g−1 for daidzein and genistein, respectively. The contents of daidzein and genistein obtained in the solid–liquid extraction were superior to 86% and 63%, respectively, compared to supercritical extraction.  相似文献   

7.
A simple dispersive liquid–liquid microextraction (DLLME) protocol for the determination of 15 organochlorine pesticides residues in honey is proposed. The selected pesticides were separated using gas chromatography and detected by electron capture (ECD) or ion trap mass spectrometry (GC-IT/MS). Several parameters affecting the extraction efficiency namely type and volume of organic extraction solvent, type and volume of disperser solvent, sample pH, ionic strength, extraction time and centrifugation speed were systematically investigated. The final DLLME protocol involved the addition of 750 μL acetonitrile (disperser) and 50 μL chloroform (extraction solvent) into a 5 mL aqueous honey solution followed by centrifugation. The sedimented organic phase (chloroform) were analysed directly by GC-IT/MS or evaporated and reconstituted in acetonitrile prior to the GC-ECD analysis. The analytical performance of the GC-ECD and GC-IT/MS methods was compared and discussed. Under the selected experimental conditions, the enrichment factors varied between of 36 and 114. The limits of detection (LOD) were in the range of 0.02–0.15 μg L−1 (0.4–3 ng g−1) for GC-ECD and 0.01–0.2 μg L−1 (0.2–4 ng g−1) for GC-IT/MS which is adequate to verify compliance of products to legal tolerances. The proposed method was applied to the analysis of the selected organochlorine pesticides residues in various honey samples obtained from Greek region. Mean recoveries were ranged from 75% to 119% while the precision was better than 20% in both methodologies.  相似文献   

8.
For the first time a method for determination of herbicides diquat (DQ) and paraquat (PQ) in olive oil was developed utilising liquid chromatography–electrospray ionization mass spectrometry (MRM). n-Hexane/10 mM HFBA aqueous solution partitioning was used as the extraction method. Separation was carried out in an Xterra C8 column (100 × 21 mm, 3 μm), using the gradient mode. Solvent A was a HFBA aqueous solution (5 mM, pH 2) and solvent B acetonitrile/methanol 75/25 (v/v). Peaks used for quantification were m/z = 157 (diquat) and m/z = 158 (paraquat). Detection limit found for both diquat and paraquat was 4 μg kg−1. The method can also be applied for determination of chlormequat (CQ, quantification peak m/z = 58), the detection limit being 0.3 μg kg−1. Such limits are clearly lower than the MCLs commonly applied to olive oil as reference criteria (5 times MCLs in olives). Good reproducibilities (day to day and run to run) were obtained.  相似文献   

9.
In order to study the content and composition of isoflavones retained in soybean seed component, obtained each component part the embryo, cotyledon and seed coat tissues of nine different soybean varieties were analyzed for 12 isoflavones using high performance liquid chromatography with photo diode array detector (HPLC-PDA) and were compared to each other. A total average concentration of isoflavone was 2887 μg g−1 in embryo, 575 μg g−1 in whole seed, 325 μg g−1 in cotyledon, and 33 μg g−1 in seed coat. With respect to each tissue of soybean varieties, isoflavone content was highest in Geomjeongkong 2 embryo (5701 μg g−1), Geomjeongolkong whole seed (1321 μg g−1), Heugcheongkong cotyledon (951 μg g−1), and Keunolkong seed coat (56 μg g−1). Isoflavone was least present in Keunolkong embryo (341 μg g−1), Hwaeomputkong whole seed (175 μg g−1), Seonheukkong cotyledon (81 μg g−1), and Seoklyangputkong seed coat (5 μg g−1). Overall, embryo and seed coat of all nine varieties contained isoflavones at the highest and lowest level, respectively. Isoflavones accumulated in the order of malonylglycoside, glycoside, acetylglycoside, and aglycon, among which malonylglycoside was the most abundant form ranging from 66% to 79% of the total isoflavone content in all three tissues. The embryo of cooked-with-rice soybean with black seed coat appears to be the best source of isoflavone.  相似文献   

10.
The solid phase extraction method developed using N-benzoyl-N-phenylhydroxylamine as a chelating reagent and Amberlite XAD-1180 as an adsorbent was used for the determination of Cu(II) and Fe(III) in various food samples by flame atomic absorption spectrometry. The samples were digested by using nitric acid and hydrogen peroxide. The Cu concentrations ranged from 1.01 to 5.81 μg g−1 in cereals, from 0.40 to 9.67 μg g−1 in vegetable and fruits and from 0.37 to 0.70 μg g−1 in infusions while the Fe concentrations ranged from 7.48 to 34.3 μg g−1 in cereals, from 5.74 to 260 μg g−1 in vegetable and fruits, from 1.63 to 5.12 μg g−1 in infusions and from 0.24 to 1.56 mg L−1 in beverage samples. The Cu and Fe concentrations found were compared with the results obtained from the other food studies in the world.  相似文献   

11.
Meadowsweet was extracted in water at a range of temperatures (60–100 °C), and the total phenols, tannins, quercetin, salicylic acid content and colour were analysed. The extraction of total phenols followed pseudo first-order kinetics, the rate constant (k) increased from 0.09 ± 0.02 min−1 to 0.44 ± 0.09 min−1, as the temperature increased from 60 to 100 °C. An increase in temperature from 60 to 100 °C increased the concentration of total phenols extracted from 39 ± 2 to 63 ± 3 mg g−1 gallic acid equivalents, although it did not significantly affect the proportion of tannin and non-tannin fractions. The extraction of quercetin and salicyclic acid from meadowsweet also followed pseudo first-order kinetics, the rate constant of both compounds increasing with an increase in temperature up until 90 °C. Therefore, the aqueous extraction of meadowsweet at temperatures at or above 90 °C for 15 min yields extracts high in phenols, which may be added to beverages.  相似文献   

12.
Carrot (Daucus carota) shoots were enriched by selenium using foliar application. Solutions of sodium selenite or sodium selenate at 10 and 100 μg Se ml−1, were sprayed on the carrot leaves and the selenium content and uptake rate of selenium were estimated by ICP–MS analysis. Anion and cation exchange HPLC were tailored to and applied for the separation of selenium species in proteolytic extracts of the biological tissues using detection by ICP–MS or ESI–MS/MS. Foliar application of solutions of selenite or selenate at 100 μg Se ml−1 resulted in a selenium concentration of up to 2 μg Se g−1 (dry mass) in the carrot root whereas the selenium concentration in the controls was below the limit of detection at 0.045 μg Se g−1 (dry mass). Selenate-enriched carrot leaves accumulated as much as 80 μg Se g−1 (dry mass), while the selenite-enriched leaves contained approximately 50 μg Se g−1 (dry mass). The speciation analyses showed that inorganic selenium was present in both roots and leaves. The predominant metabolised organic forms of selenium in the roots were selenomethionine and γ-glutamyl-selenomethyl-selenocysteine, regardless of which of the inorganic species were used for foliar application. Only selenomethionine was detected in the carrot leaves. The identity of selenomethionine contained in carrot roots and leaves was successfully confirmed by HPLC–ESI–MS/MS.  相似文献   

13.
An effective matrix solid-phase dispersion (MSPD) extraction for determination of two pyrethroids (cypermethrin and deltamethrin) in porcine tissues (liver, muscle, heart and kidney) is described. A neutral alumina-based MPSD column was used for extraction of analytes. The high-performance liquid chromatography and ultraviolet detector was applied using a reverse-phase C18 column and acetonitrile-water (85:15, v/v) was used as mobile phase. The good linear fit curve ranging from 0.05 to 50 μg mL−1 for cypermethrin (CM) and deltamethrin (DM) was obtained with a regression coefficient (r) of 0.999. Recoveries at 0.2 and 0.5 μg g−1 levels were between 83.5% and 109%. The limits of detection and quantification were: 0.01 and 0.026 μg g−1 for CM, 0.017 and 0.056 μg g−1 for DM, respectively. The proposed method was successfully applied to the determination of the pyrethroids in porcine tissues.  相似文献   

14.
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).  相似文献   

15.
Determination of phthalate sum in fatty food by gas chromatography   总被引:1,自引:0,他引:1  
Presented method for determination of sum of phthalates is based on their alkaline hydrolysis to phthalic acid at 80 °C for 20 h, followed by the selective extraction of lipophilic interferents from acidified hydrolysate at pH 1 with n-hexane. Phthalic acid is derivatized to dimethyl phthalate (DMP) with diazomethane in aqueous-chloroform two-phase system. Resulting DMP is absorbed in chloroform and determined by GC-FID. Method calibration resulted in LOD and LOQ of 0.4 (2.1) and 1.2 (6.2) μg g−1 (nmol g−1) DMP, respectively. Real samples of Baltic herring and codfish, butter, pork, goose and duck fats, sunflower, olive, rapeseed and linseed oils were analysed and the background corrected total phthalates content was found in the range from not detected level in duck fat to 12.5 (64.3) μg g−1 (nmol g−1) in butter, respectively.  相似文献   

16.
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).  相似文献   

17.
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.  相似文献   

18.
A novel, rapid and sensitive method for the simultaneous multi-channel hydride generation atomic fluorescence spectrometry (HG-AFS) determination of total arsenic (As), total bismuth (Bi), total tellurium (Te) and total selenium (Se) in tea leaves was proposed. The operating parameters of self-made multi-channel HG-AFS were optimised, including negative high voltage of photo multiplier tube (PMT), the flow rates of carrier and shield gas, observation height and lamp currents. The conditions of hydride generation for As, Bi, Te and Se were studied in details. Under optimal conditions, the method detection limits (MDL) for As, Bi, Te and Se in tea leaves were 0.0152 μg g−1, 0.0080 μg g−1, 0.0022 μg g−1 and 0.0068 μg g−1, respectively. The proposed method was successfully applied to the simultaneous determination of As, Bi, Te and Se in various tea leaves and the spike recoveries were in the range of 90–103%. The accuracy of method was validated by analysing a tea certified reference material. The obtained values were consistent with the certified ones.  相似文献   

19.
Concentrations of methylmercury (MeHg) residues were determined in different marine and freshwater fishes from Ghana. Samples were treated with ethanolic potassium hydroxide in water bath at 100 °C for 1 h. After neutralising with HCl and washing with hexane, MeHg was extracted with dithizone in toluene, cleaned up and determined by gas chromatography with electron capture detection (GC–ECD). The method was sensitive with good precision, detection limit of 0.0005 μg g−1 (0.5 μg kg−1) and provided good separation for organomercury compounds. The validity of the method was established using dogfish muscle certified reference material, DORM-2. The method was applied to different fish species. Concentration of MeHg in the edible muscle tissue of the tested fish ranged from 0.009 to 0.107 μg g−1 wet weight. The concentrations of MeHg in the fish samples obtained do not however, constitute any significant mercury exposure to the general population through consumption of the tested fish species.  相似文献   

20.
Dichloromethane, ethyl acetate, acetone, methanol, and water extracts prepared from the fruits and leaves of Laurocerasus officinalis Roem. (LO) (Rosaceae) were screened for their cholinesterase inhibitory activity against acetylcholinesterase (AChE) and butyrylcholinesterase (BChE), the key enzymes in pathogenesis of Alzheimer's disease (AD), using ELISA microplate reader at 50, 100, and 200 ??g mL−1. As AD is associated with oxidative stress, the antioxidant activity of the extracts was also tested by radical-forming methods against 2,2-diphenyl-1-picrylhydrazyl (DPPH), N,N-dimethyl-p-phenylendiamine (DMPD), and superoxide radicals as well as iron-related methods; iron-chelating capacity and ferric-reducing antioxidant power (FRAP) assays. Total phenol and flavonoid quantification was achieved using Folin-Ciocalteau and AlCl3 reagents, respectively. The highest AChE (44.01 ± 1.75%) and BChE (19.91 ± 0.37%) inhibition was caused by the LO-leaf-methanol extract 200 ??g mL−1, while it showed the best radical-scavenging activity against DPPH at 2000 ??g mL−1. Only, the dichloromethane and water extracts of the fruits and the leaf water extract had an iron-chelating capacity, while the leaf methanol extract displayed the highest FRAP. The leaf methanol extract (113.45 ± 0.71 mg g−1 extract) was found to be the richest in total phenols, while the leaf acetone extract (139.90 ± 4.64 mg g−1 extract) had the most abundant amount of total flavonoids.  相似文献   

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