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1.
高效液相色谱法检测水产品中的孔雀石绿和结晶紫   总被引：3，自引：0，他引：3  
样品中的孔雀石绿、结晶紫经试剂盒提取,浓缩后用经固相萃取柱净化、硼氢化钾还原、反向色谱柱分离,使用荧光检测器检测,孔雀石绿、结晶紫的加标回收率在76.1%～92.5%之间,相对标准偏差1.9%～5.8%,检出限均为0.5μg/kg。结果表明:该方法检测孔雀石绿(MG)、结晶紫(GV)处理简单,灵敏度高,节省时间,可用于大量样品的快速分析。  相似文献   

2.
Marine microorganisms are a new source of natural antifouling compounds. In this study, two bacterial strains, Kytococcus sedentarius QDG-B506 and Bacillus cereus QDG-B509, were isolated from a marine biofilm and identified. The bacteria fermentation broth could exert inhibitory effects on the growth of Skeletonema costatum and barnacle larvae. A procedure was employed to extract and identify the antifouling compounds. Firstly, a toxicity test was conducted by graduated pH and liquid-liquid extraction to determine the optimal extraction conditions. The best extraction conditions were found to be pH 2 and 100% petroleum ether. The EC50 value of the crude extract of K. sedentarius against the test microalgae was 236.7 ± 14.08 μg mL-1, and that of B. cereus was 290.6 ± 27.11 μg mL-1. Secondly, HLB SPE columns were used to purify the two crude extracts. After purification, the antifouling activities of the two extracts significantly increased: the EC50 of the K. sedentarius extract against the test microalgae was 86.4 ± 3.71 μg mL-1, and that of B. cereus was 92.6 ± 1.47 μg mL-1. These results suggest that the metabolites produced by the two bacterial strains are with high antifouling activities and they should be fatty acid compounds. Lastly, GC-MS was used for the structural elucidation of the compounds. The results show that the antifouling compounds produced by the two bacterial strains are myristic, palmitic and octadecanoic acids.  相似文献   

3.
An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix flowed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity （R〉0,99） in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability （RSD〈5%, n=6）. The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.  相似文献   

4.
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   

5.
The procedures of ultrasonic extraction and clean-up were optimized for the determination of polycyclic aromatic hydrocarbons (PAHs) in marine sediments. Samples were ultrasonically extracted, and the extracts were purified with a miniaturized silica gel chromatographic column and analyzed with high performance liquid chromatography (HPLC) with a fluorescence detector. Ultrasonication with methanol-dichloromethane (2:1, v/v) mixture gave higher extraction efficiency than that with dichloromethane. Among the three elution solvents used in clean-up step, dichloromethane-hexane (2:3, v/v) mixture was the most satisfactory. Under the optimized conditions, the recoveries in the range of 54.82% to 94.70% with RSDs of 3.02% to 23.22% for a spiked blank, and in the range of 61.20% to 127.08% with RSDs of 7.61% to 26.93% for a spiked matrix, were obtained for the 15 PAHs studied, while the recoveries for a NIST standard reference SRM 1941b were in the range of 50.79% to 83.78% with RSDs of 5.24% to 21.38%. The detection limits were between 0.75 ng L-1 and 10.99 ng L-1for different PAHs. A sample from the Jiaozhou Bay area was examined to test the established methods.  相似文献   

6.
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   

7.
The aim of this study was to investigate the effects of light intensity and enhanced nitrogen supply on the growth and photosynthesis of the green-tide macroalga, Ulva prolifera. Thalli of U. prolifera were grown in natural or NH 4 +-enriched seawater under two different light intensities for 7 days, and then the growth rate, pigmentation, and photosynthetic performance of the thalli were evaluated. The results show that the relative growth rate(RGR) was markedly higher under the high light level than under the low light level. Enrichment with NH 4 + enhanced the RGR under high light intensity, but did not affect RGR under low light intensity. In low light conditions, NH 4 +-enrichment resulted in a marked decrease in the maximal photosynthetic rate( P m) and the maximum carbon fixation rate( V max), but it did not affect the half saturation constant for carbon( K 0.5) or the ratio of V max to K 0.5, which reflects the carbon acquisition efficiency. In high light conditions, P m, K 0.5, and the dark respiration rate( R d) increased under NH 4 + enrichment, but V max and the V max / K 0.5 ratio decreased. Regardless of the light intensity, NH 4 +-enrichment did not affect the apparent photosynthetic efficiency( α), which refl ects the ability of the alga to use light energy at low light levels. Under both low and high light intensities, the chlorophyll a(Chl a), chlorophyll b(Chl b), and carotenoids(Car) contents in thalli were higher in NH 4 +-enriched than in natural seawater, except that there was a decrease in the Chl b content of thalli in NH 4 +-enriched seawater under low light intensity. Therefore, NH 4 + enrichment improved the growth and photosynthetic performance of U. prolifera under high light intensity, but not under low light intensity. We discuss the possible mechanisms underlying these physiological responses.  相似文献   

8.
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   

9.
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   

10.
The Henry’s Law constant (k) for phosphine in seawater was determined by multiple phase equilibration combined with headspace gas chromatography. The effects of pH, temperature, and salinity on k were studied. The k value for phosphine in natural seawater was 6.415 at room temperature (approximately 23°C). This value increases with increases in temperature and salinity, but no obvious change was observed at different pH levels. At the same temperature, there was no significant difference between the k for phosphine in natural seawater and that in artificial seawater. This implies that temperature and salinity are major determining factors for k in marine environment. Double linear regression with Henry’s Law constants for phosphine as a function of temperature and salinity confirmed our observations. These results provide a basis for the measurement of trace phosphine concentrations in seawater, and will be helpful for future research on the status of phosphine in the oceanic biogeochemical cycle of phosphorus.  相似文献   

11.
Euphausia pacific is an important source of natural astaxanthin.Studies were carried out to assess the extractability of astaxanthin from E.pacific using subcritical 1,1,1,2-tetrafluoroethane(R134a).To examine the effects of multiple process variables on the extraction yield,astaxanthin was extracted under various conditions of pressure(30-150 bar),temperature(303-343 K),time(10-50 min),flow rate(2-10 g min-1),moisture content(5.5%-63.61%),and particle size(0.25-0.109 mm).The results showed that the extraction yield increased with temperature,pressure,time and flow rate,but decreased with moisture content and particle size.A maximum yield of 87.74% was obtained under conditions of 100 bar,333 K,and 30 min with a flow rate of 6 g min-1 and a moisture content of 5.5%.The substantial astaxanthin yield obtained under low-pressure conditions demonstrates that subcritical R134a is a good alternative to CO 2 for extraction of astaxanthin from E.pacific.  相似文献   

12.
A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is established. By conditional experiments, the optimum analytical conditions and parameters are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 15-16-2 (nodes). The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviation of the calculated results for iron and manganese is 2.30% and 2.67% respectively. The results of standard addition method show that for the tap water, the recoveries of iron and manganese are in the ranges of 98.0%-104.3% and 96.5%-104.5%, and the RSD is in the range of 0.23%-0.98%; for the Yellow River water (Lijin district of Shandong Province), the recoveries of iron and manganese are in the ranges of 96.0%-101.0% and 98.7%-104.2%, and the RSD is in the range of 0.13%-2.52%; for the seawater in Qingdao offshore, the recoveries of iron and manganese are in the ranges of 95.3%-104.8% and 95.3%-104.7%, and the RSD is in the range of 0.14%-2.66%. It is found that 21 common cations and anions do not interfere with the determination of iron and manganese under the optimum experimental conditions. This method exhibits good reproducibility and high accuracy in the determination of iron and manganese and can be used for the simultaneous determination of iron and manganese in tap water and natural water. By using the established ANN- catalytic spectrophotometric method, the iron and manganese concentrations of the surface seawater at 11 sites in Qingdao offshore are determined and the level distribution maps of iron and manganese are drawn.  相似文献   

13.
The effects of various salinity fluctuation amplitudes (2, 4, 6 and 8) on the growth, osmolarity, Na+-K+-ATPase activity and Hsp70 of juvenile Fenneropenaeus chinensis cultured in seawater with a salinity of 20 were studied. The results show that weight gain in the salinity fluctuation treatments was better than that in control; in particular, the weight gain of treatments S4 and S0, at 231.8% and 196.3%, respectively, was significantly different (P<0.05). The hemolymph osmolarity of treatments S0, S2, S4, S6 and S8 was 635.4, 630.8, 623.6, 614.4 and 600.3 mOsm/kg, respectively, and decreased with increasing salinity fluctuation amplitude. The level of Na+-K+-ATPase activity in gills of F. chinensis was higher than that in hepatopancreas, but there were no significant differences among all treatments, either in gills or hepatopancreas (P>0.05). The relative level of Hsp70 in treatment S4 was 48.4% and 40.4% higher than control in muscle and eyestalks, respectively, with the highest values being recorded under a salinity fluctuation amplitude of 4.  相似文献   

14.
A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(Ⅱ)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(Ⅱ)-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 g/L. The detection limit of this method reached 0.19 g/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation (n = 7) was 1.9% for samples containing 10 g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student’s t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.  相似文献   

15.
The de-eutrophication abilities and characteristics of Ulva pertusa, a marine green alga, were investigated in Qingdao Yihai Hatchery Center from spring to summer in 2005 by analyzing the dynamic changes in NH 4 + , NO 3 ? , NO 2 ? as well as the total dissolved inorganic nitrogen (DIN). The results show that the effluent wastewater produced by fish aquaculture had typical eutrophication levels with an average of 34.3 μmol L?1 DIN. This level far exceeded the level IV quality of the national seawater standard and could easily lead to phytoplankton blooms in nature if discarded with no treatment. The de-eutrophication abilities of U. pertusa varied greatly and depended mainly on the original eutrophic level the U. pertusa material was derived from. U. pertusa used to living in low DIN conditions had poor DIN removal abilities, while materials cultured in DIN-enriched seawater showed strong de-eutrophication abilities. In other words, the de-eutrophication ability of U. pertusa was evidently induced by high DIN levels. The de-eutrophication capacity of U. pertusa seemed to also be light dependent, because it was weaker in darkness than under illumination. However, no further improvement in the de-eutrophication capacity of U. pertusa was observed once the light intensity exceeded 300 μmol M2 S?1. Results of semi-continuous wastewater replacement experiments showed that U. pertusa permanently absorbed nutrients from eutrophicated wastewater at a mean rate of 299 mg/kg fresh weight per day (126 mg/kg DIN during the night, 173 mg/kg in daytime). Based on the above results, engineered de-eutrophication of wastewater by using a U. pertusa filter system seems feasible. The algal quantity required to purify all the eutrophicated outflow wastewater from the Qingdao Yihai Hatchery Center into oligotrophic level I clean seawater was also estimated using the daily discharged wastewater, the average DIN concentration released and the de-eutrophication capacity of U. pertusa.  相似文献   

16.
Sample seawater containing trace methyl mercury was acidified and adsorbed on hydrosulfo-cotton, washed with hydrochloric acid, extracted by benzene and dried, and then determined by a gas chromatograph with electron capture detector. This method, which can detect a minimum concentration of 0.1×10−10%, can be used to monitor the 10−10% content of methyl mercury in seawater.  相似文献   

17.
The effects of different NaCl concentrations, nitrogen sources, carbon sources, and carbon to nitrogen molar ratios on biomass accumulation and polyhydroxybutyrate (PHB) production were studied in batch cultures of the marine photosynthetic bacterium Rhodovulum sulfidophilum P5 under aerobic-dark conditions. The results show that the accumulation of PHB in strain P5 is a growth-associated process. Strain P5 had maximum biomass and PHB accumulation at 2%-3% NaCl, suggesting that the bacterium can maintain growth and potentially produce PHB at natural seawater salinity. In the nitrogen source test, the maximum biomass accumulation (8.10±0.09 g/L) and PHB production (1.11±0.13 g/L and 14.62%±2.25% of the cell dry weight) were observed when peptone and ammonium chloride were used as the sole nitrogen source. NH 4 + -N was better for PHB production than other nitrogen sources. In the carbon source test, the maximum biomass concentration (7.65±0.05 g/L) was obtained with malic acid as the sole carbon source, whereas the maximum yield of PHB (5.03±0.18 g/L and 66.93%±1.69% of the cell dry weight) was obtained with sodium pyruvate as the sole carbon source. In the carbon to nitrogen ratios test, sodium pyruvate and ammonium chloride were selected as the carbon and nitrogen sources, respectively. The best carbon to nitrogen molar ratio for biomass accumulation (8.77±0.58 g/L) and PHB production (6.07±0.25 g/L and 69.25%±2.05% of the cell dry weight) was 25. The results provide valuable data on the production of PHB by R. sulfidophilum P5 and further studies are on-going for best cell growth and PHB yield.  相似文献   

18.
The acute toxicity of five phenolic compounds each to 15 d old Artemia sinica was determined in this study. The brine shrimp A. sinica was hatched from the encysted dry eggs(Bohai Bay Brand) produced by Dongying Ocean Artemia Co., Ltd., China at 27℃± 1℃ in pre-filtered(through pores of 0.45 μm in diameter) and autoclaved seawater(salinity 31, pH 7.5–8.0) in a cilindroconical glass beaker(2000 mL in volume) under continuous illumination(provided by a side set 20 W fluorescent lamp) with slight aeration. Ten Artemia individuals from the same batch of the hatched were cultured in 10 mL toxicant solution prepared with seawater(salinity 31, pH 7.5–8.0) at room temperature(about 20℃) to determine 24 h, 48 h and 72 h medium lethal concentration(LC50) of 5 phenolic compounds each. It was found that the toxicity of n-heptylphenol was the highest followed by nonylphenol, t-butylphenol, 2,4-dichlorophenol and bisphenol A in order. The LC50 values of the 5 compounds were calculated with regression analysis. The real concentration(in μg- L1) of 5 phenolic compounds each in toxicant solutions was measured with GC/MS analysis. Significant loss of phenolic compounds caused by either adsorption or desorption was not found. The significant difference of LC50 values was found among the five compounds 3 exposure times each. The range between the highest no-observed-effect concentration(NOEC) and 100% death causing concentration of five phenolic compounds each was determined. The toxicity in term of 24 h LC50 value of n-HP was 9.10 times higher than that of BPA, 1.71 times higher than t-BP, 1.53 times higher than 2,4-DCP and 1.36 times higher than NP, respectively.  相似文献   

19.
A study on the nonspecific immunity of Litopenaeus vannamei ever inhabiting freshwater and seawater was carried out at different molt stages by comparing their total hemocyte count(THC) and respiratory burst(RB) and activity of phenol oxidase(PO), nitric oxide synthase(NOS) and lysozyme(LY). Two-way ANOVA showed that salinity and molt stage independently affected THC and RB and the activity of PO, NOS and LY of juvenile L. vannamei significantly(P 0.05). The THC and RB and the activity of NOS gradually increased from the post-molt stages(A and B) to the pre-molt stages(D0–D3), which were common in shrimps inhabiting freshwater and seawater. The activity of PO peaked at the inter-molt stage(C), and touched the lowest at the post-molt stage in freshwater and pre-molt stage in seawater. The activity of LY was stable over the molt cycle. The RB and the activity of PO, NOS and LY of juvenile L. vannamei were significantly lower in freshwater than in seawater; whereas THC was significantly higher in freshwater than in seawater(P 0.05). It was concluded that the post-molt stage(especially stage A) was critical to shrimp culture, which should be intensively attended when L. vannamei was cultured in freshwater.  相似文献   

20.
This study of the petroleum hydrocarbons in coastal seawater, using dichloromethane extraction withO-terphenyl and n-C_(20) as internal standards, and gas chromatography with silica-capillary-column showedthat the recovery of petroleum hydrocarbons reaches 87.8% and that the lowest detection limit is 0.96μg.This method is reproducible, highly accurate, and applicable for determining the petroleum hydrocarbonsin coastal seawater.  相似文献   

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