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1.
This study examined levels of polycyclic aromatic hydrocarbons (PAHs) in estuarine sediments in Licun (Qingdao, China) by gas chromatography under optimized conditions for sample pretreatment via ultrasonic extraction, column chromatography, and thin layer chromatography. Methanol and dichloromethane (DCM)/methanol (2:1, v/v) were used in ultrasonic extraction, and DCM was used as eluate for column chromatography. The developing system consisted of n-hexane and DCM at a ratio of 9:1 (v/v), with DCM as the extraction solvent for PAHs-containing silica gel scraped off the plate. When the spiking level is 100 ng, total recoveries of spiked matrices for four target PAHs (phenanthrene, anthracene, pyrene and chrysene) were 83.7%, 76.4%, 85.8%, and 88.7%, respectively, with relative standard deviation (RSD) between 5.0% and 6.5% (n = 4). When the spiking level is 1000 ng, associated total recoveries were 78.6%, 72.7%, 82.7% and 85.3%, respectively, with RSD between 4.4% and 5.3% (n = 4). The opti-mized method was advantageous for determination of PAHs in complex matrix due to its effective sample purification.  相似文献   

2.
Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L~(-1) CH_3COONH_4 and 15 mmol L~(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L~(-1) for As B, 0.4261 μg L~(-1) for As(III), 0.216 μg L~(-1) for DMA, 0.211 μg L~(-1) for MMA, and 0.709 μg L~(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.  相似文献   

3.
Molecularly imprinted polymers(MIPs) were prepared by the bulk polymerization using crystal violet as the template molecule, and the methacrylic acid and ethylene glycol dimetheacrylate as functional monomer and cross-linker, respectively. Systematic investigations of synthetic conditions were conducted. The surface morphology and recognition mechanism of the obtained polymers were studied using scanning electron microscope and spectrophotometric analysis. MIPs showed high affinity to template molecule and were successfully applied as special solid-phase extraction sorbent for selective extraction of crystal violet from natural seawater. An off-line molecularly imprinted solid-phase extraction(MISPE) method followed by high-performance liquid chromatography with diodearray detection for the analysis of crystal violet was also established. MISPE columns have good recoveries for crystal violet standard solutions and good linearity was obtained over the concentration range of 0-200 μg L-1(R2 0.99). Finally, two natural seawater samples were investigated. The recoveries of spiked seawater on the MISPE columns were from 44.47% to 62.34%, the relative standard deviation(n=3) being in the range of 2.89%-5.96%.  相似文献   

4.
Phenolic compounds have become one kind of the important pollutants of the marine environment. Single-walled Carbon nanotubes, as one-dimensional nano materials, have light weight and perfect hexagonal structure of connections, with many unusual mechanical, chemical and electrical properties. In recent years, with the research of carbon nanotubes and other nano materials, the application prospect is also constantly discussed. In this paper, homemade single-walled carbon nanotubes(SWCNTs) coating was used for establishing an analytical approach to the determination of five kinds of phenolic compounds in seawater using SPME-GC-MS. Optimal conditions: After saturation was conducted with Na Cl, and p H was adjusted to 2.0 with H_2SO_4, the extract was immersed in a water bath at 40 for GC℃-MS determination through 40-min agitating extraction at 500 rmin~(-1) and 3-min desorption at 280℃. The liniearities ranged between 0.01-100 μg L~(-1), and the determination limits ranged between 1.5-10 ngL~(-1). The relative standard deviation(RSD, n = 5) was less than 6.5%. For the phenolic compounds obtained from the spiked recovery test for actual seawater samples, the rates of recovery were 87.5%-101.7%, and the RSDs were less than 8.8%, which met the requirements of determination. Due to its simplicity, high efficiency and low consumption, this approach is suitable for the analysis of trace amounts of phenolic compounds in marine waters.  相似文献   

5.
A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L~(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg~(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg~(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.  相似文献   

6.
As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg~(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.  相似文献   

7.
The toxicities of 4 common endocrine-disrupting chemicals (EDCs), 17β-estradiol (E2), p,p′-dichlorodiphenyldichloro-ethylene (DDE), 4-nonylphenol (NP) and tributyltin (TBT), to sperm motility, fertilization rate, hatching rate and embryonic development of Barbel chub (Squaliobarbus curriculus) were investigated in this study. The duration of sperm motility was significantly shortened by exposure to the EDCs at the threshold concentrations of 10 ng L?1 for E2 and TBT, 1 μg L?1 for NP and 100 μg L?1 for DDE, respectively. The fertilization rate was substantially reduced by the EDCs at the lowest observable effect concentrations (LOECs) of 10 ng L?1 for E2 and TBT and 10 μg L?1 for DDE and NP, respectively. Of the tested properties of S. curriculus, larval deformity rate was most sensitive to EDC exposure and was significantly increased by DDE at the lowest experimental level of 0.1 μg L?1. Other EDCs increased the larval deformity rate at the LOECs of 1 ng L?1 for E2, 10 ng L?1 for TBT and 1 μg L?1 for NP, respectively. Despite their decreases with the increasing EDC concentrations, the hatching rate and larval survival rate of S. curriculus were not significantly affected by the exposure to EDCs. The results indicated that all the 4 EDCs affected significantly and negatively the early life stages of the freshwater fish S. curriculus. Overall, E2 and TBT were more toxic than NP and DDE, while DDE might be more toxic to larval deformity rate than to other measured parameters. Thus, the 4 EDCs showed potential negative influences on natural population dynamics of S. curriculus. Our findings provided valuable basic data for the ecological risk assessment of E2, DDE, NP and TBT.  相似文献   

8.
The effects of four ions and eight neuroactive compounds on inducing larval settlement of A. japonicus were assessed in the present study. All bioassays were conducted in 60 × 9 mm Petri dishes, each contained 10 mL of the test solution and 10 doliolaria larvae. There were significant inductive effects of K+(10- mmol L-1), NH+4(0.1 mmol L1), GABA(10-3 mol L-1), acetylcholine(10-5 mol L-1), L-DOPA(10-5 mol L-1), norepinephrine(10-5 mol L-1) and dopamine(10-7 mol L-1 and 10-5 mol L-1) on the settlement of sea cucumber larvae. L-DOPA and dopamine are the most efficient chemical cues to induce A. japonicus larvae to settle. The highest percentage of larval settlement was induced by 10-5 mol L-1 L-DOPA and dopamine(33% and 40%) compared to the control(7%). However, Ca2+, Mg2+, choline, serotonin, and epinephrine were less effective on larval settlement at all tested concentrations. This study evaluated the stability and feasibility of chemical cues for larval settlement in different culture systems, which can be applied to improve the hatchery production of this valuable species.  相似文献   

9.
Lignin serves as one of the most important molecular fossils for tracing Terrestrial Organic Matters (TOMs) in marine environment. Extraction and derivatization of lignin oxidation products (LOPs) are crucial for accurate quantification of lignin in marine sediment. Here we report a modification of the conventional alkaline cupric oxide (CuO) oxidation method, the modification consisting in a solid phase extraction (SPE) and a novel on-column derivatization being employed for better efficiency and reproducibility. In spiking blanks, recoveries with SPE for the LOPs are between 77.84% and 99.57% with relative standard deviations (RSDs) ranging from 0.57% to 8.04% (n=3), while those with traditional liquid-liquid extraction (LLE) are from 44.52% to 86.16% with RSDs being from 0.53% to 13.14% (n=3). Moreover, the reproducibility is greatly improved with SPE, with less solvent consumption and shorter processing time. The average efficiency of on-column derivatization for LOPs is 100.8% ± 0.68%, which is significantly higher than those of in-vial or in-syringe derivatization, thus resulting in still less consumption of derivatizing reagents. Lignin in the surface sediments sampled from the south of Yangtze River estuary, China, was determined with the established method. Recoveries of 72.66% to 85.99% with standard deviation less than 0.01mg/10g dry weight are obtained except for p-hydroxyben-zaldehyde. The lignin content Σ8 (produced from 10 g dry sediment) in the research area is between 0.231 and 0.587 mg. S/V and C/V ratios (1.028 ± 0.433 and 0.192 ± 0.066, respectively) indicate that the TOMs in this region are originated from a mixture of woody and nonwoody angiosperm plants; the high values of (Ad/Al) v suggest that the TOMs has been highly degraded.  相似文献   

10.
A new kinetic spectrophotometric method has been developed for the determination of trace Ni (II) in natural water.The method is based on the catalytic effect of Ni (II) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium.The concentration of nickel (II) can be determined spectrophotometrically by measuring the decrease of absorbance of RAWL at λ= 626 nm using the fix-time method.The influencing factors are investigated by the orthogonal experimental design.The obtained optimum analytical conditions are:pH=2.00,c RAWL=5.00×10-5 mol L-1,cKIO 4= 2.00×10-5 mol L-1,the reaction time t=10 min and the temperature T=25℃..Under the optimum conditions,the developed method allows the measurement of Ni (II) in a range of 0-40.0 ng mL-1.The standard deviation of eleven independent measurements of blank reaction is S=3.08×10-3 and the limit of detection is 2.20 ng mL-1.The relative standard deviations (RSDs) in six replicate determinations of 5 ng mL-1 and 8 ng mL-1 Ni (II) are 2.87% and 1.11%,respectively.Moreover,the experiments show few cations and anions can interfere with the measurement of Ni (II).The recovery efficiencies of this method are in a range of 97.0%-102.5% in freshwater samples.But there is a decreasing effect,which is about 0.2 times the added Ni (II) in seawater medium.After reasonable calibration this processing method is used for the determination of Ni (II) in seawater samples successfully.The results show this developed method has high accuracy and precision,high sensitivity,large range of linearity and high speed.The method can,therefore,be employed at room temperature.  相似文献   

11.
This study aimed to optimize the purification of recombinant growth hormone from Paralichthys olivaceus. Recombinant flounder growth hormone (r-fGH) was expressed by Escherichia coli in form of inclusion body or as soluble protein under different inducing conditions. The inclusion body was renatured using two recovery methods, i.e., dilution and dialysis. Thereafter, the refolded protein was purified by Glutathione Sepharase 4B affinity chromatography and r-fGH was obtained by cleavage of thrombin. For soluble products, r-fGH was directly purified from the lysates by Glutathione Sepharase 4B affinity chromatography. ELISA-receptor assay demonstrated that despite its low receptor binding activity, the r-fGH purified from refolded inclusion body had a higher yield (2.605 mgL-1) than that from soluble protein (1.964 mgL-1). Of the tested recovery methods, addition of renaturing buffer (pH 8.5) into denatured inclusion body yielded the best recovery rate (17.9%). This work provided an optimized purification method for high recovery of r-fGH, thus contributing to the application of r-fGH to aquaculture.  相似文献   

12.
Marine organisms constitute unlimited resource of bioactive substances due to their high biodiversity and represent a valuable source of new compounds. This study optimized the alkali-extraction conditions and antioxidant activities of soluble polysaccharides from the body wall of Sipunculus nudus. The effects of solid-liquid ratio, extraction duration, extraction temperature, and alkali concentration on the yield of S. nudus polysaccharides (SNP) were examined, according to which the optimal combination of extraction parameters was obtained by an orthogonal test. The relative influencing importance of different extraction parameters on the yield of SNP followed the order as solid-liquid ratio > extraction temperature > alkali concentration > extraction duration. The highest extraction yield, 1.98%, was achieved under an optimal extraction condition: temperature 60°C, solid-liquid ratio 1:6 g mL?1, duration 5 h, and alkali (NaOH) mass fraction 6%. The in vitro antioxidant activities examination showed that extracted SNP under this optimized condition had strong power in reducing certain hydroxyl and superoxide radical scavenging abilities. The promising results showed that extracted SNP could be a potent natural antioxidant.  相似文献   

13.
Polycyclic aromatic hydrocarbons (PAHs) contamination of topsoil in Benxi City, Northeast China was investigated in this study, and sampling sites were located in industrial area and residential area. Results demonstrate that there is high variability in the total PAHs concentrations, ranging from 783.00 ng/g to 729 076.29 ng/g dry weight in the topsoil of Benxi City and the pollution in industrial area is the most serious. The results also present that higher molecular weight PAHs (4–6 rings) contribute substantially (79.03%) to the overall content of PAHs. The PAHs sources were determined with factor analysis by nonnegative constraints, and the results show that PAHs originating from traffic tunnel, power plant, coke oven and residential emission sources, account for 27.10%, 40.81%, 20.11% and 11.98%, respectively, of the total. The PAHs pollution is the most serious around Benxi Iron and Steel Group Corporation, and the PAHs mainly originate from coke oven and traffic tunnel, with the average contribution rate of 57.40% and 42.60%, respectively. The source apportionment results are basically consistent with the industry distribution, and the geographical and climatic characteristics of the study area.  相似文献   

14.
建立检测水产品中盐酸小檗碱残留量的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经酸化甲醇(含体积分数1%甲酸)提取,正己烷脱脂,离心后,用高效液相色谱-串联质谱仪分析。以选择反应监测(SRM)正离子模式分析,定性离子对为336/320和336/292,定量离子对为336/320,盐酸小檗碱质量浓度在1~100 ng/mL范围内线性关系良好,线性相关系数为0.999 7,检出限为0.001 mg/kg。样品盐酸小檗碱的添加剂量为5~100μg/kg时,平均加标回收率为81.29%~104.06%,相对标准偏差为2.97%~7.87%,可满足水产品中盐酸小檗碱残留检测和药代动力学的研究需要。  相似文献   

15.
The distributions of particulate and dissolved dimethylsulfoxide(DMSOp, DMSOd) were studied for the first time in the surface water of the South China Sea(SCS) in January 2010. The concentrations of DMSOp ranged from 2.6 to 56.8 nmol L~(-1) with an average of 11.1 ± 2.2 nmol L~(-1), and those of DMSOd ranged from 11.8 to 335.1 nmol L~(-1) with an average of 50.0 ± 16.5 nmol L~(-1). DMSOd dominated over both dimethylsulfide(DMS) and dissolved dimethylsulfoniopropionate(DMSPd) by 1–3 orders of magnitude and represented the major dissolved dimethyl sulfur pool. In addition, DMSOp/chlorophyll-a ratios varied from 2.7 to 180.7 mmol g~(-1) with an average of 30.5 ± 9.6 mmol g~(-1). DMSOd concentrations displayed a significant negative relationship with sea surface temperature(SST) and sea surfaces salinity(SSS) in the whole study area. The distribution of DMSOd in the coastal waters was obviously influenced by the Pearl River discharge, with high concentrations appearing around the river mouth. In the offshore waters, a significant correlation was observed between the DMSOp and DMSOd concentrations, suggesting that DMSOd was mainly from the diffusion of intracellular DMSO rather than from the photochemical and biological oxidation of DMS.  相似文献   

16.
The application of soxhlet, ultrasonic and accelerated solvent extraction techniques to the analysis of six organochlorine pesticides (α-HCH, β-HCH, γ-HCH, o, p'-DDT, p,p'-DDT and p, p'-DDE) in Taihu Lake sediment samples is described. It was found that the limits of quantification ranged from 0.002μgg-1 to 0.004μgg-1, and the recoveries of organochlorine pesticides with the three extraction techniques were acceptable (>80.7%). With a mass selective detector, better results were obtained by accelerated solvent extraction using hexane-acetone (1:1) as compared with soxhlet and ultrasonic extraction. It was shown that the accelerated solvent extraction was the optimum technique for the analysis of organochlorine pesticides in sediments. The general features of the three extraction techniques are also presented.  相似文献   

17.
A full life-cycle toxicity test, combined with histology, on calanoid copepod Schmackeria poplesia was used to study the effect of bis(tributyltin) oxide (TBTO). The results indicate no sex-specific differences in TBTO toxicity. Long-term mortalities of the copepods exposed to concentrations higher than 20 ng TBTO L−1 were significantly elevated compared with that of control, and larval development was inhibited when they were exposed to 40 and 60 ng TBTO L−1. The percentages of ovigerous females were reduced compared with the control (P<0.01) after 24 days exposure to concentrations higher than 10 ng TBTO L−1. Histological examinations suggest that exposure to TBTO might block the posterior end of the diverticula and inhibits the production of egg sacs. A modified Euler-Lotka equation was used to calculate a population-level endpoint, the intrinsic rate of natural increase (r m), from individual life-table endpoints, i.e. mortality rate, time of release of first brood, sex ratio, the fraction of ovigerous females among all females as well as the number of nauplii per ovigerous female. Apart from the highest TBTO concentration (60 ng L−1), where all females aborted their egg sacs, 20 ng TBTO L−1 was the only concentration that significantly decreased r m compared with that of control (an effect associated with decreased sex ratio). The results show that the S. poplesia is affected by prolonged exposure to low concentrations of TBTO. The full life-cycle toxicity test combined with histology experiments provides more integral understanding of the toxicity of endocrine disrupters.  相似文献   

18.
A total of 348 species belonging to 8 phyla and 125 genera were observed in seasonally sampled phytoplankton of tidal rivers from 13 sampling sites around Luoyuan Bay, and all field samplings were carried out in productive period(March/June/August/December) at ebb tide. Bacillariophyta species were the most abundant species, followed by Chlorophyta, Cyanophytes, Euglenophyta, Cryptophyta, Dinophyta, Xanthophyta and Chrysophytas. Seasonal distribution index(SDI) value ranged from 0.63 to 0.86, which meant that species found at those sites in 4 seasons tended to be largely different. Phytoplankton individuals ranged from 5.939×10~4 ind L~(-1) in winter to 75.31×10~4 ind L~(-1) in autumn. Phytoplankton biomass ranged from 0.620 mg L~(-1) in summer to 2.373 mg L~(-1) in autumn. The grey correlation analysis(GCA) showed that the nutrient variables played an important role in the influence on phytoplankton community in every season. The canonical correspondence analysis(CCA) revealed impact of environmental variables on the different species, most of Bacillariophyta species were negative correlation with nutrients(TP and NH_3-N) in the four seasons, Chlorophyta species and Cyanophyta species did not show obvious correlation with environment variables in every season. The combination of GRA analysis and CCA analysis provided a method to quantitatively reveal the correlation between phytoplankton community and environmental variables in water body of tidal rivers at this region.  相似文献   

19.
Bacteria of the genus Flammeovirga can digest complex polysaccharides (CPs), but no details have been reported regarding the CP depolymerases of these bacteria. MY04, an agarolytic marine bacterium isolated from coastal sediments, has been identified as a new member of the genus Flammeovirga. The MY04 strain is able to utilize multiple CPs as a sole carbon source and grows well on agarose, mannan, or xylan. This strain produces high concentrations of extracellular proteins (490 mg L-1 ± 18.2 mg L-1 liquid culture) that exhibit efficient and extensive degradation activities on various polysaccharides, especially agarose. These proteins have an activity of 310 U mg-1 ± 9.6 U mg-1 proteins. The extracellular agarase system (EAS) in the crude extracellular enzymes contains at least four agarose depolymerases, which are with molecular masses of approximately 30-70 kDa. The EAS is stable at a wide range of pH values (6.0-11.0), temperatures (0-50℃), and sodium chloride (NaCl) concentrations (0- 0.9 mol L-1). Two major degradation products generated from agarose by the EAS are identified to be neoagarotetraose and neoagarohexaose, suggesting that β-agarases are the major constituents of the MY04 EAS. These results suggest that the Flammeovirga strain MY04 and its polysac-charide-degradation system hold great promise in industrial applications.  相似文献   

20.
The vertical distributions and sources of PAHs in sediment of Xiamen Bay   总被引:2,自引:0,他引:2  
INTRODUCTIONTheindustrialdevelopmentandrisingpopulationintheXiamencoastalzonearelikelytoresultinincreasingpollutantsloadingwhichcanaffecttheoceanicecosystemsenvironmentthereandthreatenhumanhealth .PAHs ,asgoodenvironmentpollutionindicators(Aizenshat,1 973 ;Randahl,1 983 ) ,arerela tivelystableinairandwater,andarewidelydistributedintheaquaticenvironmentasaresultofhumanactivities.ProposedprimarysourcesofPAHsincludecombustionofvariousfossilfuels,nat uralfires,roadrunoff streetdustaswellas…  相似文献   

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