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1.
A vortex-assisted liquid–liquid microextraction (VALLME) method using hexanoic acid as extractant followed by high-performance liquid chromatography–diode array detection was developed for the extraction and determination of five phthalate esters (PAEs) including bis-methylglycol ester (DMEP), benzyl butyl phthalate (BBP), dicyclohexyl phthalate (DCHP), di-n-butyl phthalate (DBP), and di-n-octyl phthalate (DNOP) from liquor samples. In this method, hexanoic acid was employed as extraction solvent, because its density is lower than water. And vortex mixing was utilized as a mild emulsification procedure to reduce emulsification time and improve the effect of extraction. Under the studied conditions, five phthalate esters were successfully separated within 20 min and the limits of detection were 2.3 ng mL?1 for DMEP, 1.1 ng mL?1 for BBP, 1.9 ng mL?1 for DCHP, 1.2 ng mL?1 for DBP, and 1.5 ng mL?1 for DNOP, respectively. Recoveries of the PAEs spiked into liquor samples were ranged from 89 to 93 %. The precisions of the proposed method were varied from 1.6 to 2.6 % (RSD). The VALLME method has been proved to have the potential to be applied to the preconcentration of the target analytes. Moreover, the method is simple, high sensitivity, consumes much less solvent than traditional methods and environmental friendly.  相似文献   

2.
A new analytical method by graphene-reinforced hollow fiber liquid-phase microextraction combined with high-performance liquid chromatography fluorescence detection was developed for the determination of bisphenol A and 4-tert-butylphenol in bottled juices. Several important experimental parameters were studied to get optimal extraction conditions for the analytes. Under the optimized conditions, the method showed a good performance having a linear response in the range from 0.05 to 10.0 ng mL?1 with the correlation coefficients (r) of 0.9965–0.9994 and limits of detection of 0.01 ng mL?1. The relative standard deviations were in the range from 6.4 to 7.2 % at the spiked concentration of 1.0 ng mL?1. The method combines the high-adsorption capacity of graphene and the excellent clean-up performance of hollow fiber liquid-phase microextraction and has been successfully applied to the analysis of the analytes in bottled juice samples.  相似文献   

3.
Sudan dyes are often illegally added as colorants into a variety of foodstuffs and have been tied to many food safety issues. In this study, surface-enhanced Raman spectroscopy (SERS) coupled with Au–Ag core-shell nanospheres (Au@Ag) was applied to analyze standard solutions of Sudan I–IV and Sudan dyes in chili flakes. With the use of 90 ± 5 nm Au@Ag (Au seed 20 ± 2 nm) as SERS substrate, the lowest detectible concentrations for Sudan I and II were 0.10 mg/L, for Sudan III was 0.08 mg/L, and for Sudan IV was 0.2 mg/L. The use of principal component analysis (PCA) could successfully classify different Sudan dyes based upon the SERS spectra of their standard solutions. For chili flakes, the use of acetonitrile as extraction solvent led to an overall higher sensitivity for analysis of Sudan dyes with SERS method compared to that of methanol, ethanol, and n-hexane. The lowest detectible concentrations for Sudan I–III in chili flakes were 1 mg/kg and for Sudan IV was 2 mg/kg, which were about ten times as much as that for their standard solutions due to the interference of non-target compounds from sample matrices. Partial least squares (PLS) models developed for quantitative analyses showed relatively high linear correlation between the actual and predicted amounts of Sudan dyes in chili flakes (R 2 cv = 0.869–0.959). The results showed great potential of applying Au@Ag as SERS substrate for qualitative and quantitative analysis of Sudan I–IV with simplified sample preparation method.  相似文献   

4.
In this work a simple, rapid and sensitive method using dispersive liquid–liquid microextraction (DLLME) combined with UV–Vis spectrophotometry has been developed for the preconcentration and determination of trace amounts of aziridine in food simulants. The method is based on derivatization of aziridine with Folin's reagent (1,2-naphthoquione-4-sulphonic acid) and extraction of color product using DLLME technique. Some important parameters, such as reaction conditions, and type and volume of extraction solvent and disperser solvent were studied and optimized. Under optimum conditions, a linear calibration curve in the range of 2.0–350 ng mL?1 of aziridine was obtained. Detection limit based on 3Sb was 1.0 ng mL?1, and the relative standard deviation for 50 ng mL?1 of aziridine was 2.49c (n?=?7). The proposed method was applied for the determination of aziridine in food simulants.  相似文献   

5.
In this project, a simple, low-cost and rapid procedure based on dispersive liquid–liquid microextraction (DLLME) technique coupled with high performance liquid chromatography-ultraviolet detector (HPLC-UV) has been used for the extraction and determination of styrene in aqueous solutions. Several factors, such as type of extraction and dispersive solvents and their volumes, salt addition, and pH were optimized. Under optimal conditions, the recoveries of styrene for tea and water samples spiked with 10 and 15 ng mL?1 were in the range of 91.4–97.8 %, whereas the temperature was set at 0, 4, 20, 70 and 91 °C for 15, 30, 60, 1440, and 14,400 min. The linear range was obtained in the interval of 1.86–50 ng mL?1. The limits of detection (S/N = 3) and quantitation (S/N = 10) were 0.6 and 1.86 ng mL?1, respectively. The relative standard deviations (RSDs) for three replicated analysis of styrene in aqueous samples ranged from 0.01 to 0.3 %.  相似文献   

6.
A combination of dispersive micro solid-phase extraction (DMSPE), based on graphene as a solid sorbent, with energy dispersive X-ray fluorescence spectrometry (EDXRF) is proposed for preconcentration and determination of Co(II), Ni(II), and Cu(II) ions in wine samples. In the developed procedure, cupferron complexes of metal ions are adsorbed on graphene dispersed in aqueous samples. After the adsorption process, aqueous samples are passed through a membrane filter with the use of filtration assembly, and then loaded filters are directly measured using EDXRF. In order to obtain high recovery of the metal ions, various analytical parameters influencing sorption were optimized, such as pH, amount of graphene, Triton X-100 and cupferron, sample volume, and sorption time. Under optimal conditions, the calibration plots cover the 2 to 100 ng mL?1 range for Co(II) and Ni(II), and 2 to 150 ng mL?1 for Cu(II). The detection limits of 0.08, 0.08, and 0.07 ng mL?1 for Co(II), Ni(II), and Cu(II) were obtained using 50 mL sample volume and 200 μg of graphene. The precision (at a 20 ng mL?1 level for n?=?10) is lower than 3.5 %. The proposed method was successfully applied to determination of Co, Ni, and Cu in wine samples.  相似文献   

7.
The affinity reaction between the antibodies to okadaic acid immobilized on the sensor’s surface and the toxin in the solution has been investigated. The affinity constant, as well as the association rate constant and the dissociation rate constant, has been calculated. The unlabeled affinity sensor for the detection of okadaic acid has been developed. The calibration plot is linear in the range of concentrations of 5–500 ng mL?1; the limit of detection is 1.4 ng mL?1. The developed sensor can be successfully used for the detection of toxins in real samples.  相似文献   

8.
Aflatoxins are a major class of fungal toxins that have food safety importance due to their economic and health impacts. This pilot aflatoxin exposure biomonitoring study on 84 individuals was conducted in a rural (Ilumafon) and a semi-urban community (Ilishan Remo) of Ogun state, Nigeria, to compare aflatoxin exposures among the two population cohorts. First morning urine samples were obtained from the participants, and the urinary aflatoxin M1 (AFM1) levels were measured by a quantitative Helica Biosystems Inc. ELISA kit assay. About 99% (83 out of 84) of the urine samples had detectable AFM1 levels in the range of 0.06 to 0.51 ng mL?1 (median: 0.27 ng mL?1). The mean urinary AFM1 levels were significantly (= 0.001) higher in the semi-urban population (0.31 ± 0.09 ng mL?1) compared to the rural population (0.24 ± 0.07 ng mL?1). There were, however, no significant differences in mean urinary AFM1 levels of males and females, and among children, adolescents and adults. This study indicates high aflatoxin exposure to the extent of public health concerns in the studied populations. Thus, more efforts are required for aflatoxin exposure monitoring and control in high-risk regions.  相似文献   

9.
Salbutamol (SAL), a kind of β-agonist which can enhance the lean meat-to-fat ratio, has been inhibited as an additive used in animal feeds for livestock production in many countries due to its harmful effect to the consumers. In this study, an ultrasensitive and specific competitive immunochromatographic test (ICT) integrated with surface-enhanced Raman scattering (SERS) for the detection of SAL was described. The immunoprobe was prepared by immobilizing polyclonal antibody against SAL on the surface of Au@Ag nanoparticles in which the Raman reporter (4-mercaptobenzoic acid, MBA) had been sandwiched. After ICT procedures, the specific SERS signals generated from MBA on the test line of the ICT strip were measured for the quantitative determination of SAL. The assay was completed in 15 min. The IC50 and the limit of detection (LOD) values of the assay for SAL were 0.028 ng mL?1 and 3.0 pg mL?1, respectively. There was no cross-reactivity (CR) of the assay with other three β-agonists (clenbuterol, phenylethanolamine A, and ractopamine), showing high specificity of the assay. Spiking experiments indicated that the average recoveries (n?=?3) of SAL from swine feed, meat, and urine samples were in ranges of 98.4–105.2 % with the relative standard deviations (RSDs) of 1.7–7.8 %. The results demonstrated that the proposed ICT was a feasible method for ultrasensitive and specific detection SAL in swine feed, meat and urine samples, and could be extended for the detection of other target analytes.  相似文献   

10.
This research was conducted to prove that developed silver biopolymer nanoparticle substrate for surface enhanced Raman scattering (SERS) technique could detect and differentiate three different serotypes of Salmonella. Nanoparticle was prepared by adding 100 mg of silver nitrate to a 2 % polyvinyl alcohol solution, then adding 1 % trisodium citrate to reduce silver nitrate and produce silver encapsulated biopolymer nanoparticles. Then, nanoparticle was deposited on a stainless steel plate and used as SERS substrate. Fresh cultures of Salmonella typhimurium, Salmonella enteritidis and Salmonella infantis were washed and suspended in 10 mL of sterile deionized water. Approximately 5 μl of the bacterial suspensions were placed on the substrate individually and exposed to 785 nm laser excitation. SERS spectral data were recorded between 400 and 1,800 cm?1. SERS signals were collected from 15 different spots on the substrate for each sample. PCA model was developed to classify Salmonella serotypes. PC1 identified 92 % of the variation between the Salmonella serotypes, and PC2 identified 6 % and in total 98 % between the serotypes. Soft independent modeling of class analogies of validation set gave an average correct classification of 92 %. Comparison of the SERS spectra of Salmonella serotypes indicated that both isolates have similar cell walls and cell membrane structures which were identified by spectral regions between 520 and 1,050 cm?1. However, major differences were detected in cellular genetic material and proteins between 1,200 and 1,700 cm?1. SERS with silver biopolymer nanoparticle substrate could be a promising tool in pathogen detection and it would potentially be used to classify them.  相似文献   

11.
Amaranth (E 123) is a member of azo dyes, and it is allowed to use in various foods. The acceptable maximum addition of amaranth is strictly fixed because of its potential risk to physical health. The objective of this study was to prepare a specific anti-amaranth monoclonal antibody and develop an indirect competitive ELISA for amaranth quantification analysis. The immunogen and the coating antigen were designed by introducing a carboxyl group into amaranth for the conjugation with carrier proteins. Based on the immunogen, the monoclonal antibody exhibits satisfactory performances and the proposed ELISA shows an IC50 of 20.33 ng mL?1. The limit of detection is as low as 3.35 ng mL?1, and the linear standard curve of the method ranges from 3.0 to 243.0 ng mL?1. Additionally, the antibody reflects minimal cross-reactivity (<1 %) with six related food dyes (erythrosine, ponceau 4R, allura red, tartrazine, sunset yellow FCF, and brilliant blue). The recoveries of amaranth spiked beverage samples are in the range of 85.8–100.7 % with low coefficient of variation values (<11.5 %). The data shows that the developed ELISA provides a simple, sensitive, specific, and accurate alternative for amaranth determination and monitoring. Furthermore, it is the first time that icELISA of amaranth is developed based on monoclonal antibodies.  相似文献   

12.
Electromembrane extraction (EME) as a novel sample preparation technique was firstly applied for the purification and enrichment of bromate (BrO3 ?) in drinking water prior to capillary zone electrophoresis with capacitively coupled contactless conductivity detection (CZE-C4D). BrO3 ?, as the primary disinfection by-product of ozonation, could be well separated with the major inorganic anions coexisting in water samples using a 300 mmol L?1 acetic acid solution as the running buffer. Under the optimum conditions, the calibration curve showed good linearity (r 2?=?0.996), and the limit of detection was down to 0.12 ng mL?1 with the enrichment factor at 267. The relative standard deviation (RSD) values for peak area and migration time at a spiked concentration of 10 ng mL?1 of bromate were below 8.8 and 2.5 %, respectively. This proposed EME-CZE-C4D method has been successfully applied to analyze bottled drinking water and tap water samples with recoveries in the range of 85~98 %, providing an alternative to the determination of bromate in drinking water.  相似文献   

13.
A novel method based on ultrasound-assisted surfactant-enhanced emulsification microextraction (UASEME) has been developed for the preconcentration of cobalt prior to its determination by graphite furnace atomic absorption spectrometry. In the UASEME technique, chloroform was used as the extraction solvent, sodium dodecyl sulfate was adopted as emulsifier, and ultrasound was applied to assist emulsification. There is no need of using organic dispersive solvent which is typically required in conventional dispersive liquid–liquid microextraction method. Several parameters that affect the extraction efficiency, such as the kind and volume of the extraction solvent, the type and concentration of the surfactant, pH of sample solution, concentration of the chelating agent, and extraction time and temperature were investigated and optimized. Under the optimal conditions, the linearity of calibration curve was in the range of 0.1–5 ng mL?1 with a correlation coefficient (R 2) of 0.9992. An enrichment factor of 58 was achieved with a sample volume of 5.0 mL. The detection limit of this method for Co was 15.6 ng L?1, and the relative standard deviation (RSD) was 4.3 % at 1.0 ng mL?1 concentration level of Co. The accuracy of the developed method was evaluated by analysis of the certified reference materials GBW07605 tea leaf and GBW10015 spinach. The method was successfully applied to determine trace cobalt in food and water samples with satisfactory results.  相似文献   

14.
Synergistic stacking technique by combining field-amplified sample injection with moving chemical reaction boundary was developed for the sensitive determination of two major sialic acids, N-acetylneuraminic acid (NANA) and N-glycolylneuraminic acid (NGNA) based on capillary electrophoresis with capacitively coupled contactless conductivity detection. A series of experimental parameters affecting electrophoretic separation, detection sensitivity, and hydrolysis efficiency of sialic acids were investigated. Under the optimum conditions, NANA and NGNA could be well separated from the common monosaccharides and disaccharides as well as other potential coexisting inorganic and organic anions in a running buffer of 30 mmol L?1 NaOH–10 mmol L?1 Na2HPO4/0.8 mmol L?1 CTAB. This developed method has been applied to determine the target analytes in dairy products. In terms of its high sensitivity (LODs 1.7–2.2 ng mL?1, namely, 5.5–7.2 nmol L?1), good linearity (r > 0.999), acceptable recovery (93–107%), and reliability of acid hydrolysis step, this proposed method provides a simple, rapid, sensitive, and environmentally friendly alternative for the analyses of the main sialic acids in dairy products without derivatization.  相似文献   

15.
In the present study, a rapid, simple, and highly efficient sample preparation method based on ion-pair air-assisted liquid–liquid microextraction using a low-density extraction solvent followed by high performance liquid chromatography–diode array detection has been developed for the extraction, preconcentration, and determination of three phthalic acids (phthalic acid, iso-phthalic acid, and terephthalic acid) in aqueous samples. In this method, a mixture of tri-butyl amine (as an ion-pair reagent) and toluene (as an extraction solvent) is transferred into an aqueous sample solution. Fine organic solvent droplets are formed by aspirating and dispersing of the mixture via syringe needle. After that, the formed ion-pairs are extracted into toluene, and after centrifuging, the obtained collected phase is transferred into a microtube and is evaporated to dryness under a stream of nitrogen at room temperature. The residue is re-dissolved in mobile phase and injected into the separation system for analysis. Under the optimum extraction conditions, the method showed low limits of detection and quantification between 0.09–0.24 and 0.29–0.78 ng mL?1, respectively. Extraction recoveries and enrichment factors were from 88 to 98 % and 443 to 491, respectively. Relative standard deviations for the extraction of 5 ng mL?1 of each analyte were less than 8.4 % for intra-day (n?=?6) and inter-days (n?=?5) precisions. Finally, different aqueous samples were successfully analyzed using the proposed method, and the target analytes were determined in some of them at ng mL?1 level.  相似文献   

16.
An accurate, sensitive spectrofluorimetric method was developed to determine 1-naphthylacetic acid and thiabendazole simultaneously in fruits in a simple, expeditious manner. Broadband overlap between the conventional spectra of the two compounds was resolved by using first-derivative constant-wavelength synchronous fluorescence spectrometry. The proposed method is based on the intrinsic fluorescence of the two agrochemicals in ethanol. The sensitivity and selectivity of the determination were optimized by examining the influence of various factors on the fluorescence intensity. Based on the results, analyses were performed in 30% (v/v) ethanol–water mixtures at a pH 4.7 adjusted with sodium citrate buffer. Using the derivative signals at 304 and 286 nm for 1-naphthylacetic acid and thiabendazole, respectively, provided linear calibration graphs over the range 10–100 and 30–120 ng mL?1, and limits of detection of 1.99 and 0.17 ng mL?1, respectively. The analytical figures of merit of the proposed method were calculated in the light of the error propagation theory. The sensitivity, repeatability, reproducibility and limits of detection obtained are acceptable for determining the two agrochemicals in strawberry tree berries and citrus fruits without the need for a time-consuming prior separation. The proposed method is simple, reliable and cost-efficient, which makes it an attractive choice for fast selective screening purposes.  相似文献   

17.
This work describes a novel sorbent based on functionalization of magnetic nanoparticles by 2-aminobenzothiazole and its application in the extraction and preconcentration of trace amount of Cd(II), Cu(II), and Ni(II) ions. This nanosorbent was characterized by Fourier transfer infrared spectroscopy, thermal analysis, X-ray powder diffraction, elemental analysis, and scanning electron microscopy. The effects of various factors such as pH value, sorption time, sorbent dosage, type, volume, and concentration of the eluent as well as the elution time were investigated. Following the sorption and the elution of target analytes, the Cd(II), Cu(II), and Ni(II) ions were determined by flame atomic absorption spectrometry. Under the optimal conditions, the limits of detection (LODs) were 0.03, 0.009, and 0.1 μg L?1 for Cd(II), Cu(II), and Ni(II), respectively. Linearity was within the range of 0.1–75 ng mL?1 for Cd(II), 0.03–50 ng mL?1 for Cu(II), and 0.5–100 ng mL?1 for Ni(II) in the initial solution with r 2 values greater than 0.9978. The relative standard deviations of the method were less than 8.4 %. The preconcentration factor of the method was 277. The sorption capacity of this new sorbent was 65, 78, and 49 mg g?1 for Cd(II), Cu(II), and Ni(II), respectively. The proposed method was validated using two certified reference materials (LGC 6010 hard drinking water and NIST SRM 1515 apple leaves) in order to exhibit its applicability. Ultimately, this method was applied to the rapid extraction of the trace quantities of Cd(II), Cu(II), and Ni(II) ions in different food samples, and satisfactory results were obtained.  相似文献   

18.
Phenylethanolamine A (PEA), a new alternative β-agonist, has been illegally used in farming to promote the muscle growth in food-producing animals. In this study, a sensitive and convenient competitive indirect enzyme-linked immunosorbent assay (ciELISA) was developed for determination of PEA residues in pork samples. The produced antibody was highly specific to PEA and exhibited a negligible cross-reactivity toward some other β-agonists. The developed technique was characterized by the limit of detection below 0.08 μg kg?1 and the IC50 value of 0.93 pmol mL?1 (0.32 ng mL?1). Validation of the technique was done using artificially spiked and naturally contaminated pork samples. The recoveries ranged from 79.6 to 112.6 % for the samples spiked at levels of 0.1–5 μg kg?1 with the variation coefficients below 15 %. The analysis of naturally contaminated samples showed that the obtained data corresponded with the data obtained by the LC-MS/MS. The developed ciELISA was shown to be a feasible highly sensitive and specific screening tool for PEA residue analysis.  相似文献   

19.
A multi-class, multi-residue analytical method based on LC-MS/MS detection was developed for the screening and confirmation of 28 veterinary drug and metabolite residues in flatfish, shrimp and eel. The chosen veterinary drugs are prohibited or unauthorised compounds in Korea, which were categorised into various chemical classes including nitroimidazoles, benzimidazoles, sulfones, quinolones, macrolides, phenothiazines, pyrethroids and others. To achieve fast and simultaneous extraction of various analytes, a simple and generic liquid extraction procedure using EDTA-ammonium acetate buffer and acetonitrile, without further clean-up steps, was applied to sample preparation. The final extracts were analysed by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The method was validated for each compound in each matrix at three different concentrations (5, 10 and 20 ng g–1) in accordance with Codex guidelines (CAC/GL 71-2009). For most compounds, the recoveries were in the range of 60–110%, and precision, expressed as the relative standard deviation (RSD), was in the range of 5–15%. The detection capabilities (CCβs) were below or equal to 5 ng g–1, which indicates that the developed method is sufficient to detect illegal fishery products containing the target compounds above the residue limit (10 ng g–1) of the new regulatory system (Positive List System – PLS).  相似文献   

20.
Chilean consumer preferences include foods that may contain considerable amounts of furan, a potential human carcinogen. However, there is no information regarding dietary exposure to furan in Chile. Thus, the objective of this work was to determine the Chilean exposure to dietary furan. To accomplish this objective, the furan concentration of 14 types of commercial foods processed at high temperature were analysed based on a modified headspace-GC/MS (HS-GC/MS) method in which the limits of detection for different food matrices ranged from 0.01 to 0.6 ng g?1. In addition, a risk assessment was made with exposure estimates based on dietary data from national studies on different age groups (9-month-old babies, school children, adults and elderly people). Of the food items surveyed “American”-type coffee (espresso coffee plus hot water) obtained from automatic coffee machine (936 ng g?1) and low moisture starchy products like crisps and “soda”-type crackers showed the highest furan concentrations (259 and 91 ng g?1, respectively). Furthermore, furan was also found in samples of breakfast cereals (approximately 20 ng g?1), jarred fruit baby foods (8.5 ng g?1) and orange juice (7.0 ng g?1). School children (aged 9–13 years) represented the highest intake of furan (about 500 ng kg?1bw day?1), with margins of exposure of 2479 and 2411, respectively, which points to a possible public health risk.  相似文献   

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