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1.
固相微萃取-气相色谱法测定水中痕量有机氯农药   总被引:3,自引:0,他引:3  
建立了固相微萃取-气相色谱联用快速测定水中14种痕量有机氯农药的方法,对比研究了浸入式直接固相微萃取与顶空固相微萃取两种方式对不同有机氯农药的富集效率,优化了试验条件.方法线性关系良好,检出限为0.1 ng/L~10 ng/L,定量下限为0.2 ng/L~40 ng/L,RSD<8%,实际水样的加标回收率为67.0%~133%.  相似文献   

2.
采用C 18柱固相萃取(SPE)-三重四级杆气相色谱-质谱法同时测定水中18种含有机氯的环境内分泌干扰物,方法在0.500μg/L^100μg/L范围内线性良好,方法检出限为0.04 ng/L^0.8 ng/L,空白水样的加标回收率为61.3%~108%,6次测定结果的RSD为3.8%~18.0%。将该方法用于饮用水源水监测,18种目标化合物的测定值为未检出~1.5 ng/L,平均加标回收率为71.9%~109%,平行测定结果的RSD<15%。  相似文献   

3.
建立了盘式固相萃取?超高效液相色谱?串联质谱快速测定地表水中n?壬基酚、双酚A、n?辛基酚的方法。1L水样经过Φ47 mm的C18盘式固相萃取膜盘萃取净化,用二氯甲烷/甲醇(体积比1∶1)洗脱、浓缩定容至1 mL。采用Waters BEH C18色谱小柱,以甲醇?0?1%氨水溶液为流动相,梯度洗脱分离后,UPLC?MS/MS多级监测模式( MRM)下以外标法进行定性定量分析。该方法检出限:双酚A为1 ng/L,n?壬基酚为0?1 ng/L,n?辛基酚为0?1 ng/L。对同一环境样品进行了3种质量浓度(5、50、200 ng/L)的加标回收实验,平均回收率为84?6%~118?8%,相对标准偏差为1?8%~8?3%。基于该方法,对巢湖入湖河流水样进行了检测,质量浓度为13?2~42?3 ng/ L。  相似文献   

4.
采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)建立了地表水中25种抗生素类药物和8种非抗生素类药物的分析方法。通过重点优化质谱参数、色谱条件、样品pH、洗脱溶剂组成及用量等确定了最佳分析条件。水样经过滤、固相萃取柱富集净化后,选择Shim-pack XR-ODS为色谱柱,以乙腈和0.2%甲酸-2 mmol/L乙酸铵-水溶液为流动相进行梯度洗脱,采用电喷雾电离源,在多反应监测模式下(MRM)分析测定,内标法定量。33种药物的仪器定量限为0.012~4.68 ng/L,方法检出限为0.011~7.60 ng/L,地表水加标回收率为53.7%~122%,相对标准偏差为1.22%~32.1%(n=6)。方法成功应用于北京市凉水河12个地表水样分析,共检出32种药物,检出质量浓度为未检出~239 ng/L。利托那韦(RTV)作为新型冠状病毒诊疗方案中推荐的药物在凉水河检出率为100%。  相似文献   

5.
建立了固相萃取(SPE)-超高效液相色谱/三重四极杆串联质谱(UPLC-MS/MS)同时测定地表水中8种亚硝胺类化合物的方法。水样中目标物经椰壳活性炭固相萃取小柱吸附富集,小柱经氮气吹干后采用二氯甲烷洗脱。待测样品采用Atlantis T3柱,以水-甲醇作为流动相进行梯度洗脱,大气压力化学电离源(APCI)正离子模式多反应监测方式(MRM)进行检测,内标法定量分析。8种目标物在相关线性范围内线性良好(r≥0.9950),地表水加标回收率为55.4%~90.4%,相对标准偏差为3.1%~14.3%,方法检出限为1.1 ~1.8 ng/L。本方法准确度和灵敏度高,适用于快速测定地表水中8种亚硝胺类化合物含量。  相似文献   

6.
通过优化固相萃取和液相色谱条件,建立了固相萃取-高效液相色谱-质谱法测定水中双酚A的检测方法。水样经C_(18)固相萃取柱净化并富集双酚A后,采用C_(18)反相色谱柱XR-ODS(2.0 mm×100 mm,2.2μm)分离,MRM负离子模式测定。结果表明:BPA浓度为5~200 ng/L范围内线性关系良好(相关系数为0.999 9),取样量500 mL,浓缩500倍时,方法检出限(LOD)和定量下限(LOQ)分别为2.0、8.0 ng/L。实际水样加标量为5、20 ng水平时,BPA的相对标准偏差(RSD,n=8)分别为8%和7%,回收率范围分别为82%~103%和90%~111%。  相似文献   

7.
建立了同位素稀释-液相色谱-串联质谱法(LC-MS/MS)同时测定养殖水体中23种镇静剂残留的方法。样品经0.45 μm滤膜过滤后,用Oasis HLB固相萃取柱净化,浓缩后用50%的甲醇水定容。以1%甲酸水溶液和乙腈为流动相,采用Agilent InfiniityLab Poroshell 120 SB-C18色谱柱分离后,在多反应监测模式下测定,内标法定量。结果表明,23种镇静剂在0.5~100ng/L质量浓度范围内线性关系良好(r>0.99),检出限和定量限分别为0.1~0.3和0.4 ~1.0 ng/L。加标回收率为73.5%~117.6%,相对标准偏差(RSD)为1.1%~9.9%。该方法前处理简单,净化效果较好,灵敏度较高,适用于池塘养殖水体中23种镇静剂类药物残留的快速检测。  相似文献   

8.
建立了地表水中9种性激素的固相萃取-超高效液相色谱-串联质谱检测方法。利用HLB固相萃取柱富集水体中痕量性激素,用甲醇洗脱并浓缩,再以1 mmol/L氟化铵-乙腈为流动相,经C_(18)柱分离,采用电喷雾离子源、质谱多反应监测模式,内标法定量,实现了地表水中9种性激素的同时检测。方法检出限为0. 1~1. 8 ng/L,在低、中、高3个加标水平下,性激素的平均回收率为69. 6%~115. 0%,相对标准偏差为3. 2%~17. 7%。该方法灵敏度高,定性准确,操作简单高效,适用于地表水中9种性激素的定性定量分析。  相似文献   

9.
固相萃取-液相色谱-串联质谱法测定水中5种雌激素   总被引:1,自引:1,他引:0       下载免费PDF全文
建立了固相萃取-液相色谱-串联质谱组合联用技术同时测定地表水、饮用水和污水处理厂出厂水中的5种雌激素(17β-雌二醇、雌三醇、雌酮、17α-炔雌醇、己烯雌酚)的方法。水样经过全自动固相萃取仪富集,以OASIS HLB柱为萃取柱,甲醇为洗脱剂,用液相色谱-串联四极杆质谱联用仪分析定量。分别在0.5~8、5~80μg/L范围内线性良好,相关系数为0.995~0.998。17β-雌二醇、雌三醇、17α-炔雌醇的检出限均为5μg/L,雌酮与己烯雌酚的检出限为0.5μg/L。5种雌激素的纯水加标回收率为63.6%~120.2%,地表水加标回收率为59.8%~91.5%,自来水加标回收率为55.3%~92.1%,精密度为3.7%~10.7%,该方法简单、可靠,可用于水中雌激素类污染物的同时测定。  相似文献   

10.
水样酸化过滤后用Oasis HLB固相萃取小柱净化富集,采用液相色谱-串联质谱法同时测定地表水中微囊藻毒素(MC-LR和MC-RR),通过优化试验条件,使方法在1.00μg/L~100μg/L范围内线性良好。MC-LR和MC-RR在水中的方法检出限为0.12 ng/L和0.2 ng/L,空白加标回收率为72.7%~88.5%,3次测定结果的RSD为9.1%~10.7%。将该方法用于6个海河流域部分重要水源地水样的监测,虽然部分水样中检测出MC-LR和MC-RR,但检出值均低于标准限值。  相似文献   

11.
An important research area in life sciences is devoted to modeling, prediction, and dynamics of gene-expression patterns. As clearly understood in these days, this enterprise cannot become satisfactory without acknowledging the role of the environment. To a representation of past, present, and most likely future states, we also encounter measurement errors and uncertainties. This paper surveys and improves recent advances in understanding the foundations and interdisciplinary implications of the newly introduced gene–environment networks, and it integrates the important theme of carbon dioxide emission reduction into the networks and dynamics. We also introduce some operational and managerial issues of practical working and decision making, expressed in terms of sliding windows, quadrants (modules) of parametric effects, and navigating (controlling) between such effects and directing them. Given data from DNA microarray experiments and environmental records, we extract nonlinear ordinary differential equations that contain parameters that have to be determined. For this, we employ modern (Chebychevian) approximation and (generalized semi-infinite) optimization. After this is provided, time- discretized dynamical systems are studied. A combinatorial algorithm with polyhedra sequences allows to detect the region of parametric stability. Finally, we analyze the topological landscape of gene–environment networks with its structural (in)stability. By embedding as a module and investigating CO2 emission control and figuring out game theoretical aspects, we conclude. This pioneering work is theoretically elaborated, practically devoted to health care, medicine, education, living conditions, and environmental protection, and it invites the readers to future research.   相似文献   

12.
In this article a comprehensive approach for the evaluation of possible health effects in an environmental impact assessment (EIA) is described, illustrated with the example of Amsterdam Airport Schiphol. Unlike many EIAs, we estimated quantitatively the impact of aircraft-related pollution in terms of the number of affected people for aircraft noise annoyance, odour annoyance and hypertension. In addition, an analysis of health registry data on cardiovascular and respiratory diseases and a short survey on annoyance and risk perception were carried out. The scope of a health impact assessment depends on the situation, available knowledge and data, concern in the population about the impact and the number of people concerned. It is important to pay attention to the perception of risks and concerns from all parties involved. Moreover, the results demonstrate that far more people outside the area for which standards apply were affected than inside.  相似文献   

13.
The San Francisco Bay estuary isused by over one million shorebirds during springmigration and is home to several hundred thousandduring the winter. Most shorebird use occurs in thesouthern reach of the estuary (South Bay). Thereduced water circulation and discharge fromindustrial sources in the South Bay are responsiblefor the highest levels of some trace elements in theestuary. Wintering shorebirds have been found to havestrong site fidelity to areas as small as a fewkilometers in the South Bay, which may increase theirexposure to contaminants near local point sources. Inaddition, different shorebird species foraging at thesame site have been shown to have differentcontaminant burdens. Thus, our objectives were totest whether contaminant burdens differed by species,or whether contaminant burdens differed in shorebirdscollected at adjacent sites. We examined thecontaminant profiles of two species of shorebirds,long-billed dowitchers (Limnodromus scolopaceus)and western sandpipers (Calidris mauri) thatforage together at two sites, Hayward and Newark,separated by 8 km in the South Bay. We usedmultivariate analysis of variance tests to compare thecomposition of 14 elemental analytes in their livertissues and estimated their molar ratios of Hg and Se. Composite samples were used for contaminant analysesbecause of the small body size of the shorebirds. Seven elemental analytes (Ag, Ba, Be, Cr, Ni, Pb, V)were below detection limits in a majority of thesamples so statistical analyses were precluded. Inthe measurable analytes (As, Cd, Cu, Hg, Mn, Se, Zn),we found no significant intra-site differences ofcontaminant profiles for the two species. We pooledthe samples to examine inter-site differences andfound significant differences in contaminant profilesbetween shorebirds at the neighboring sites (P = 0.03). Shorebirds at Newark had higher (P < 0.05) concentrations of As, Cd, and Se than those at Hayward. Dowitchers at Newark had concentrations of Hg and Se which were highly correlated (P < 0.003) in a mean molar ratio of 1:19, similar tothat reported in other birds. In the larger dowitcherspecies, we also examined exposure to 20organochlorine compounds. Organic analyses showedthat the dowitchers had been exposed to DDE, PCBs,dieldrin and trans-nonachlor, but with no significantdifferences in concentrations between Hayward andNewark (P > 0.05).  相似文献   

14.
土壤和底泥中砷、铬、锰测定的前处理技术   总被引:6,自引:0,他引:6  
试验了土壤和底泥中砷的前处理技术,其目的是能对土壤、底泥中砷、铬、锰在一次前处理中制备成试液,比色法分析。试验表明,用H2SO4-H3PO4-H2O2进行前处理是可行的。方法简单、挥发酸雾少,用标准参考物质检验证明,分解完全,数据准确,有粒较好一致性。  相似文献   

15.
Material Disposal Area G is the primary low-levelradioactive waste disposal site at Los Alamos NationalLaboratory, New Mexico, and is adjacent to Pueblo of SanIldefonso lands. Pueblo residents and Los Alamos scientists areconcerned about radiological doses resulting from uptake of AreaG radionuclides by mule deer (Odocoileus hemionus) andRocky Mountain elk (Cervus elaphus), then consumption ofdeer and elk meat by humans. Tissue samples were collected fromdeer and elk accidentally killed near Area G and were analyzedfor 3H, 90Sr, total U, 238Pu, 239, 240Pu,241Am, and 137Cs. These data were used to estimatehuman doses based on meat consumption of 23 kg y-1. Humandoses were also modeled using RESRAD, and dose rates to deer andelk were estimated with a screening model. Dose estimates tohumans from tissue consumption were 2.9 × 10-3 mSv y-1and 1.6 × 10-3 mSv y-1 from deer and elk, respectively,and RESRAD dose estimates were of the same order of magnitude. Estimated dose rates to deer and elk were 2.1 × 10-4 mGyd-1 and 4.7 × 10-4 mGy d-1, respectively. Allestimated doses were significantly less than established exposurelimits or guidelines.  相似文献   

16.
This paper presents the chemical speciation and retention behavior of chromium (Cr), nickel (Ni), and cadmium (Cd) prior to and after the electrokinetic remediation in glacial till soil. The speciation of the metals was predicted using the chemical speciation program MINEQL+. The simulations were performed for single-contaminant with only Cr(VI) or Ni, and multi-contaminants consisting of: (1) Cr(VI), Ni, and Cd; (2) Cr(III), Ni and Cd; (3) Cr(VI), Cr(III), Ni and Cd; (4) Cr(VI), Ni, and Cd with reducing agents; and (5) Cr(III), Ni, and Cd with oxidizing agent (Mn). The results showed that the speciation and distribution of cationic metals [Ni, Cd, and Cr(III)] in glacial till soil remain unaffected or slightly affected during electrokinetics. This is attributed to the high pH buffering capacity of the glacial till, leading the metals to precipitate in the soil prior to and after electrokinetics. This study showed that during electrokinetics, Cr(VI) existed as anionic complex and migrated towards the anode and the migration is maximum in case of a single-contaminant system. The study also showed that near the anode in the absence of any reducing and oxidizing agent, Cr(VI) mostly adsorbed, and some of Cr(VI) reduced to Cr(III) and migrated towards the cathode and finally precipitated due to high pH conditions. Ni and Cd remain adsorbed or precipitated due to the high pH conditions throughout the soil. Among the reducing agents, the sulfide had significant effect on the migration of metals compared to ferrous ions. While in the presence of oxidizing agent (Mn), no noticeable Cr(VI) was found in the soil sample indicating the reduction of Cr(VI) to Cr(III) and the predominance of reducing conditions due to the presence of naturally occurring iron in the glacial till soil. Overall, this study provides a reasonable explanation of the speciation and distribution of chromium, nickel and cadmium during the electrokinetic remediation of glacial till soil.  相似文献   

17.
We evaluated exposure of aquatic biota to lead (Pb), zinc (Zn), and cadmium (Cd) in streams draining a Pb-mining district in southeast Missouri. Samples of plant biomass (detritus, periphyton, and filamentous algae), invertebrates (snails, crayfish, and riffle benthos), and two taxa of fish were collected from seven sites closest to mining areas (mining sites), four sites further downstream from mining (downstream sites), and eight reference sites in fall 2001. Samples of plant biomass from mining sites had highest metal concentrations, with means 10- to 60-times greater than those for reference sites. Mean metal concentrations in over 90% of samples of plant biomass from mining sites were significantly greater than those from reference sites. Mean concentrations of Pb, Zn, and Cd in most invertebrate samples from mining sites, and mean Pb concentrations in most fish samples from mining sites, were also significantly greater than those from reference sites. Concentrations of all three metals were lower in samples from downstream sites, but several samples of plant biomass from downstream sites had metal concentrations significantly greater than those from reference sites. Analysis of supplemental samples collected in the fall of 2002, a year of above-average stream discharge, had lower Pb concentrations and higher Cd concentrations than samples collected in 2001, near the end of a multi-year drought. Concentrations of Pb measured in fish and invertebrates collected from mining sites during 2001 and 2002 were similar to those measured at nearby sites in the 1970s, during the early years of mining in the Viburnum Trend. Results of this study demonstrate that long-term Pb mining activity in southeast Missouri has resulted in significantly elevated concentrations of Pb, Cd, and Zn in biota of receiving streams, compared to biota of similar streams without direct influence of mining. Our results also demonstrate that metal exposure in the study area differed significantly among sample types, habitats, and years, and that these factors should be carefully considered in the design of biomonitoring studies.  相似文献   

18.
19.
The present study demonstrates comparison of Cr accumulatingpotential by the plants of Najas indica Cham. (submerged),Vallisneria spiralis L. (rooted submerged) and Alternanthera sessilis R. Br. (rooted emergent) under repeatedmetal exposure and its effect on chlorophyll and protein concentrations. These plants were treated with different concentrations of Cr under repeated exposure in controlled laboratory conditions to assess the maximum metal accumulationpotential. The plants of V. spiralis accumulated significantly high amount of Cr under laboratory conditions incomparison to N. indica and A. sessilis. The maximumaccumulation of 1378, 458 and 201 g g-1 dw Cr was found in the leaves of V. spiralis, N. indica and A. sessilis, respectively at 8 mg L-1 after 9 day of Cr exposure. These plants have shown a decrease in chlorophyll andprotein concentrations with increase in Cr concentrations. In view of high accumulation of Cr in V. spiralis, the plantswere treated with different concentrations of tannery effluent collected from Common Effluent Treatment Plant, Unnao (UP). Theplants of V. spiralis treated with 100% tannery wastewatershowed the maximum accumulation (57.5 g g-1 dw) of Cr in the roots after 10 days of exposure. The plants were foundeffective in removing Cr from solution and tannery effluent.  相似文献   

20.
Public transport in Delhi was amended by the Supreme Court of India to use Compressed Natural Gas (CNG) instead of diesel or petrol. After the implementation of CNG since April 2001, Delhi has the highest fraction of CNG-run public vehicles in the world and most of them were introduced within 20 months. In the present study, the concentrations of various criteria air pollutants (SPM, PM10, CO, SO2 and NOx) and organic pollutants such as benzene, toluene, xylene (BTX) and polycyclic aromatic hydrocarbons (PAHs) were assessed before and after the implementation of CNG. A decreasing trend was found for PAHs, SO2 and CO concentrations, while the NOx level was increased in comparison to those before the implementation of CNG. Further, SPM, PM10, and BTX concentrations showed no significant change after the implementation of CNG. However, the BTX concentration demonstrated a clear relation with the benzene content of gasoline. In addition to the impact of the introduction of CNG the daily variation in PAHs levels was also studied and the PAHs concentrations were observed to be relatively high between 10 pm to 6 am, which gives a proof of a relation with the limited day entry and movement of heavy vehicles in Delhi.  相似文献   

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