Pub Date : 2000-11-01DOI: 10.1051/ANALUSIS:2000280793
R. Thibaut, A. Jumel, L. Debrauwer, E. Rathahao, L. Lagadic, J. Cravedi
In order to better assess the risk associated with nonylphenol, a lipophilic contaminant of the aquatic environment having a strong tendency to bioaccumulate in organisms and exerting estrogenic effects in fish and invertebrates, we have investigated the capability of three types of freshwater species to metabolize labelled 4-n-nonylphenol. Reverse-phase radio-HPLC was used to isolate and quantify the metabolites. The identification of residues was based on co-chromatography with available standards or authenfified metabolites and when possible by electrospray ionization LC-MS analyses. The residues found in rainbow trout (Oncorhynchus mykiss), pond snails (Lymnea stagnalis) and duckweeds (Lemna minor) were identified. These freshwater organisms are able to extensively biotransform 4-n-nonylphenol. Our attempts to draw the metabolic pathways of nonlyphenol evidenced oxidative attack on the alkyl chain with the production of several hydroxylated compounds and related carboxylic acids. In addition, trout and duck-weeds were able to conjugate the phenol moiety to glucuronic acid and carbohydrates respectively. Traces of sulphate conjugates were also detected in trout tissues whereas no conjugate was detected in pond snails.
{"title":"Identification of 4-n-nonylphenol metabolic pathways and residues in aquatic organisms by HPLC and LC-MS analyses","authors":"R. Thibaut, A. Jumel, L. Debrauwer, E. Rathahao, L. Lagadic, J. Cravedi","doi":"10.1051/ANALUSIS:2000280793","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000280793","url":null,"abstract":"In order to better assess the risk associated with nonylphenol, a lipophilic contaminant of the aquatic environment having a strong tendency to bioaccumulate in organisms and exerting estrogenic effects in fish and invertebrates, we have investigated the capability of three types of freshwater species to metabolize labelled 4-n-nonylphenol. Reverse-phase radio-HPLC was used to isolate and quantify the metabolites. The identification of residues was based on co-chromatography with available standards or authenfified metabolites and when possible by electrospray ionization LC-MS analyses. The residues found in rainbow trout (Oncorhynchus mykiss), pond snails (Lymnea stagnalis) and duckweeds (Lemna minor) were identified. These freshwater organisms are able to extensively biotransform 4-n-nonylphenol. Our attempts to draw the metabolic pathways of nonlyphenol evidenced oxidative attack on the alkyl chain with the production of several hydroxylated compounds and related carboxylic acids. In addition, trout and duck-weeds were able to conjugate the phenol moiety to glucuronic acid and carbohydrates respectively. Traces of sulphate conjugates were also detected in trout tissues whereas no conjugate was detected in pond snails.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"33 1","pages":"793-801"},"PeriodicalIF":0.0,"publicationDate":"2000-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81503891","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-11-01DOI: 10.1051/ANALUSIS:2000155
R. Pöykiö, H. Torvela, P. Perämäki, T. Kuokkanen, H. Rönkkömäki
Most analytical methods for trace element determination in plant material require decomposition of the sample. Sample decomposition procedures play an important role in ensuring that chemical analysis gives correct results. This is especially im por- tant in the determination of trace elements in plant material for environmental studies because, as a rule, plant material is not homogeneous and usually contains variable matrices. In this paper microwave digestion procedures using HNO 3, HNO3+H2O2, HNO3+HClO4, HF mixtures and dry ashing + HF were investigated for the analysis of Al, Ca, Cr, K, Mg, Mn, Zn, S, Pb, V, Cu, Cd, Co and Ni by ICP-AES or ICP-MS from pine needle samples. Reference samples BCR CRM 100 (Spruce Needles), BCR CRM 101 (Beech Leaves) and HUMH2 (Organic surface soil) were used to test the dissolution methods. The results showed that the sample digestion procedure is critical step for obtaining accurate results. Losses of volatile metals were notable in many cases when dry ashing was used.
{"title":"Comparison of dissolution methods for multi-element analysis of some plant materials used as bioindicator of sulphur and heavy metal deposition determined by ICP-AES and ICP-MS","authors":"R. Pöykiö, H. Torvela, P. Perämäki, T. Kuokkanen, H. Rönkkömäki","doi":"10.1051/ANALUSIS:2000155","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000155","url":null,"abstract":"Most analytical methods for trace element determination in plant material require decomposition of the sample. Sample decomposition procedures play an important role in ensuring that chemical analysis gives correct results. This is especially im por- tant in the determination of trace elements in plant material for environmental studies because, as a rule, plant material is not homogeneous and usually contains variable matrices. In this paper microwave digestion procedures using HNO 3, HNO3+H2O2, HNO3+HClO4, HF mixtures and dry ashing + HF were investigated for the analysis of Al, Ca, Cr, K, Mg, Mn, Zn, S, Pb, V, Cu, Cd, Co and Ni by ICP-AES or ICP-MS from pine needle samples. Reference samples BCR CRM 100 (Spruce Needles), BCR CRM 101 (Beech Leaves) and HUMH2 (Organic surface soil) were used to test the dissolution methods. The results showed that the sample digestion procedure is critical step for obtaining accurate results. Losses of volatile metals were notable in many cases when dry ashing was used.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"35 1","pages":"850-854"},"PeriodicalIF":0.0,"publicationDate":"2000-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82633188","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-11-01DOI: 10.1051/ANALUSIS:2000152
H. Sabik, R. Jeannot, E. Sauvard
The stability of 18 herbicides (ten organonitrogens and eight phenylureas, including four degradation products), selected for the frequency of their detection in the environment, was evaluated under a variety of storage conditions. Large volumes of s ur- face water (4 L) were extracted using large-particle-size graphitized carbon black cartridges (Carbopack B 60-80 mesh). The effe cts of temperature, matrix type, drying and solvent-washing of cartridges on the recovery of these contaminants, after different stora ge periods, were studied and compared to the conservation of surface water in bottles. After two months, there was no significant di ffer- ence between the conserved surface water and the stored cartridges for the selected compounds. Cartridges kept at -20 °C were be t- ter than those stored at 4 °C and 20 °C. The type of matrix water selected, in this case St. Lawrence surface water, appears to hav e a minor effect on the recovery of the target pesticides after cartridge storage. No improvement was observed in the recovery of a ny of the chemicals when the cartridges were dried or washed and stored in a solvent. After immediate surface-water extraction, the mo st practical storage condition for the target herbicides was found to be storage on cartridges in the dark at - 20 °C, with no solven t dry- ing or washing of the Carbopack B material.
选取了18种除草剂(10种有机氮类和8种苯脲类，包括4种降解产物)，根据其在环境中的检测频率，对其在不同储存条件下的稳定性进行了评价。使用大粒径石墨化炭黑墨盒(carbpack B 60-80目)提取大体积(4l)的表面水。研究了温度、基质类型、干燥和溶剂洗涤对不同贮存期后这些污染物回收的影响，并与瓶中地表水的保存进行了比较。两个月后，保存的地表水和储存的样品中所选化合物的含量没有显著差异。保存在-20°C的墨盒比保存在4°C和20°C的墨盒效果更好。所选择的基质水类型，在本例中是圣劳伦斯地表水，似乎对药筒储存后目标农药的回收率影响不大。当墨盒干燥或洗涤并储存在溶剂中时，没有观察到任何化学物质的回收。经直接地表水提取后，发现目标除草剂最实用的储存条件是在- 20°C的黑暗环境中储存在墨盒中，不需要对Carbopack B材料进行溶剂干燥或洗涤。
{"title":"Stability of herbicides and their degradation products on graphitized carbon black extraction cartridges used for large volumes of surface water","authors":"H. Sabik, R. Jeannot, E. Sauvard","doi":"10.1051/ANALUSIS:2000152","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000152","url":null,"abstract":"The stability of 18 herbicides (ten organonitrogens and eight phenylureas, including four degradation products), selected for the frequency of their detection in the environment, was evaluated under a variety of storage conditions. Large volumes of s ur- face water (4 L) were extracted using large-particle-size graphitized carbon black cartridges (Carbopack B 60-80 mesh). The effe cts of temperature, matrix type, drying and solvent-washing of cartridges on the recovery of these contaminants, after different stora ge periods, were studied and compared to the conservation of surface water in bottles. After two months, there was no significant di ffer- ence between the conserved surface water and the stored cartridges for the selected compounds. Cartridges kept at -20 °C were be t- ter than those stored at 4 °C and 20 °C. The type of matrix water selected, in this case St. Lawrence surface water, appears to hav e a minor effect on the recovery of the target pesticides after cartridge storage. No improvement was observed in the recovery of a ny of the chemicals when the cartridges were dried or washed and stored in a solvent. After immediate surface-water extraction, the mo st practical storage condition for the target herbicides was found to be storage on cartridges in the dark at - 20 °C, with no solven t dry- ing or washing of the Carbopack B material.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"68 1","pages":"835-842"},"PeriodicalIF":0.0,"publicationDate":"2000-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80279187","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-11-01DOI: 10.1051/analusis:2000156
H. Aboul‐Enein, X. Sun
A novel ion selective PVC membrane electrode for determination of propranolol is developed. Silicotungstic acid is used as the counter ion and diisononyl phthalate (DNP) used as the plastizer. The electrode exhibits excellent potential respon se properties, showing a Nernstian response in the concentration of 3.0 〈 10-6~ 2.6 〈 10-2 M with the slope of 54.7 mV per decade, shorter conditioning time (~ 3 h), fast response time (40 s), a lower limit of detection (1.0 〈 10-7 M). The electrode is success- fully used for the analysis of propranolol in pharmaceutical formulation with the recoveries of 99.2 ~ 102.6 %, by using a direct potentiometric method and which does not require tedious sample preparation.
{"title":"A novel ion selective PVC membrane electrode for determination of propranolol in pharmaceutical formulation","authors":"H. Aboul‐Enein, X. Sun","doi":"10.1051/analusis:2000156","DOIUrl":"https://doi.org/10.1051/analusis:2000156","url":null,"abstract":"A novel ion selective PVC membrane electrode for determination of propranolol is developed. Silicotungstic acid is used as the counter ion and diisononyl phthalate (DNP) used as the plastizer. The electrode exhibits excellent potential respon se properties, showing a Nernstian response in the concentration of 3.0 〈 10-6~ 2.6 〈 10-2 M with the slope of 54.7 mV per decade, shorter conditioning time (~ 3 h), fast response time (40 s), a lower limit of detection (1.0 〈 10-7 M). The electrode is success- fully used for the analysis of propranolol in pharmaceutical formulation with the recoveries of 99.2 ~ 102.6 %, by using a direct potentiometric method and which does not require tedious sample preparation.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"48 1","pages":"855-858"},"PeriodicalIF":0.0,"publicationDate":"2000-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78709374","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-11-01DOI: 10.1051/ANALUSIS:2000147
J. Száková, P. Tlustoš, J. Balík, D. Pavlíková, M. Balíková
Various soil extraction methods were developed for the determination of total and/or plant-available concentrations of potentially toxic elements. In this experiment, four single extraction procedures ( aqua regia, HNO3, acetic acid, DTPA) were tested for the determination of extractable contents of As, Cd and Zn. 35 soils differing in their physicochemical properties an d in total element contents were used in this experiment. Extractability of elements from soil samples varied following the indi- vidual elements and/or extraction agents used. The strong acids were not able to release the elements tightly bound into the si l- icate sample matrix. However, such techniques remain utilizable for the approximate determination of "pseudototal" element con- tents in soil, especially if soil samples are affected by anthropogenic contamination. The concentrations of As, Cd, and Zn determined in soil extracts by both mineral and organic acids covered in most cases the element portion representing more than one soil element fraction determined using SM&T sequential extraction procedure. Solutions of acetic acid and DTPA were able to release a part of the element fraction bound in Fe/Mn oxides and organic matter of soil sample. Arsenic represents an excep- tion because it is not released by DTPA.
{"title":"Efficiency of extractants to release As, Cd and Zn from main soil compartments.","authors":"J. Száková, P. Tlustoš, J. Balík, D. Pavlíková, M. Balíková","doi":"10.1051/ANALUSIS:2000147","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000147","url":null,"abstract":"Various soil extraction methods were developed for the determination of total and/or plant-available concentrations of potentially toxic elements. In this experiment, four single extraction procedures ( aqua regia, HNO3, acetic acid, DTPA) were tested for the determination of extractable contents of As, Cd and Zn. 35 soils differing in their physicochemical properties an d in total element contents were used in this experiment. Extractability of elements from soil samples varied following the indi- vidual elements and/or extraction agents used. The strong acids were not able to release the elements tightly bound into the si l- icate sample matrix. However, such techniques remain utilizable for the approximate determination of \"pseudototal\" element con- tents in soil, especially if soil samples are affected by anthropogenic contamination. The concentrations of As, Cd, and Zn determined in soil extracts by both mineral and organic acids covered in most cases the element portion representing more than one soil element fraction determined using SM&T sequential extraction procedure. Solutions of acetic acid and DTPA were able to release a part of the element fraction bound in Fe/Mn oxides and organic matter of soil sample. Arsenic represents an excep- tion because it is not released by DTPA.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"1 1","pages":"808-812"},"PeriodicalIF":0.0,"publicationDate":"2000-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72822131","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-11-01DOI: 10.1051/ANALUSIS:2000280783
M. Solé, M. Castillo, M. Alda, C. Porte, D. Barceló
In a laboratory experiment, adult male and female carp, Cyprinus carpio, were intraperitoneally injected with a single dose of 500 μg/kg of 17α-ethynylestradiol (EE 2 ) and eight days afterwards, vitellogenin levels were recorded in blood by Western blot analysis. Moreover, effects on the cytochrome P450 monooxygenase system, phase II and antioxidant defense enzymes of the liver were measured. In a field approach, water and carp were simultaneously collected at the vicinity of two sewage treatment works (STWs) for determining the presence of estrogenic compounds such as nonylphenol (NP) and nonylphenol polyethoxylated compounds (NPEOs) as well as the occurrence of natural and sinthetic estrogens. The induction of vitellogenin on the male individuals was used as a reliable indicator of estrogenic exposure.
{"title":"Estrogenicity determination in carp, Cyprinus carpio: a laboratory and field approach","authors":"M. Solé, M. Castillo, M. Alda, C. Porte, D. Barceló","doi":"10.1051/ANALUSIS:2000280783","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000280783","url":null,"abstract":"In a laboratory experiment, adult male and female carp, Cyprinus carpio, were intraperitoneally injected with a single dose of 500 μg/kg of 17α-ethynylestradiol (EE 2 ) and eight days afterwards, vitellogenin levels were recorded in blood by Western blot analysis. Moreover, effects on the cytochrome P450 monooxygenase system, phase II and antioxidant defense enzymes of the liver were measured. In a field approach, water and carp were simultaneously collected at the vicinity of two sewage treatment works (STWs) for determining the presence of estrogenic compounds such as nonylphenol (NP) and nonylphenol polyethoxylated compounds (NPEOs) as well as the occurrence of natural and sinthetic estrogens. The induction of vitellogenin on the male individuals was used as a reliable indicator of estrogenic exposure.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"71 1","pages":"783-788"},"PeriodicalIF":0.0,"publicationDate":"2000-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90644666","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-11-01DOI: 10.1051/ANALUSIS:2000158
J. Surlève‐Bazeille, M. Mercier, R. Tarroux, A. Mavon, E. Neuzil, D. Licu, P. Dupuy
This paper is the first application of scanning electron microscopy (SEM) and of energy dispersive selection micro- analysis (EDS) to the study of natural spa waters used as sprays in current dermatological practice; the aim was to relate the mineral composition of the spray to the sensitory perception recorded by the patients. Crystallized deposits were first obtaine d on a collodion film, from two spa waters mainly containing hydrogenocarbonate, calcium and magnesium ions, but differing by their Mg/Ca ratio. In order to understand the types of crystals formed, mineral solutions of simpler composition were prepared and submitted to the same process. Among the crystalline varieties of calcium carbonate, calcite and vaterite were characterized ; aragonite could not be detected in spa waters deposits, despite the presence of magnesium, which favours the crystallization of this orthorhombic form in the artificial solutions.
{"title":"Scanning electron microscopy and energy dispersive spectrometric microanalysis of crystalline deposits following evaporation of CO$_3$H$^-$, Mg$^{2+}$ and Ca$^{2+}$ containing aqueous solutions","authors":"J. Surlève‐Bazeille, M. Mercier, R. Tarroux, A. Mavon, E. Neuzil, D. Licu, P. Dupuy","doi":"10.1051/ANALUSIS:2000158","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000158","url":null,"abstract":"This paper is the first application of scanning electron microscopy (SEM) and of energy dispersive selection micro- analysis (EDS) to the study of natural spa waters used as sprays in current dermatological practice; the aim was to relate the mineral composition of the spray to the sensitory perception recorded by the patients. Crystallized deposits were first obtaine d on a collodion film, from two spa waters mainly containing hydrogenocarbonate, calcium and magnesium ions, but differing by their Mg/Ca ratio. In order to understand the types of crystals formed, mineral solutions of simpler composition were prepared and submitted to the same process. Among the crystalline varieties of calcium carbonate, calcite and vaterite were characterized ; aragonite could not be detected in spa waters deposits, despite the presence of magnesium, which favours the crystallization of this orthorhombic form in the artificial solutions.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"11 1","pages":"864-871"},"PeriodicalIF":0.0,"publicationDate":"2000-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89117078","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-10-01DOI: 10.1051/ANALUSIS:2000143
M. Couprie, J. Ortega
The free-electron laser ("FEL") has proven to be an invaluable source of radiation in the UV to far infrared spectral ranges. It is based on the amplification of an optical wave by a high energy electron beam oscillating transversely to its prop a- gation. In the last decade, several FELs have been designed and built as user dedicated facilities. Presently, seven infrared FEL s, such as CLIO at Orsay (France), are running more than 1000 hours/year for users performing experiments in various scientific fields. In the UV spectral range, the Super-ACO (Orsay, France) FEL is promoting applications in various fields. The main appli- cations are described and prospects are given.
{"title":"Free-electron lasers sources for scientific applications","authors":"M. Couprie, J. Ortega","doi":"10.1051/ANALUSIS:2000143","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000143","url":null,"abstract":"The free-electron laser (\"FEL\") has proven to be an invaluable source of radiation in the UV to far infrared spectral ranges. It is based on the amplification of an optical wave by a high energy electron beam oscillating transversely to its prop a- gation. In the last decade, several FELs have been designed and built as user dedicated facilities. Presently, seven infrared FEL s, such as CLIO at Orsay (France), are running more than 1000 hours/year for users performing experiments in various scientific fields. In the UV spectral range, the Super-ACO (Orsay, France) FEL is promoting applications in various fields. The main appli- cations are described and prospects are given.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"28 1","pages":"725-736"},"PeriodicalIF":0.0,"publicationDate":"2000-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91029458","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-10-01DOI: 10.1051/ANALUSIS:2000142
N. Carro, I. García, M. Llompart
A reliable and simple procedure to extract polychlorinated biphenyls (PCBs) from marine mussels using microwave energy is proposed. Freeze-dried mussels were subjected to MASE (Microwave Assisted Solvent Extraction) in a closed-vessel microwave system with n-pentane-sodium hydroxide (5 %) or dichloromethane-pentane (1:1) at different temperatures (70 and 90 oC), the extraction time was 10 minutes. Sample extract cleanup procedure was performed by using alumina. Gas chromatog- raphy-mass spectrometry and gas chromatography-electron capture detector were employed for individual congener identification and determination. The influence of the following variables on microwave extraction of PCBs has been studied: extraction tem- perature, solvent volume, solvent nature, cleanup procedure time and volume of sodium hydroxide solution. Recoveries for PCBs were between 77 and 106 % with relative standard deviation between 2 to 20 %. Validation of the extraction process was carried out by processing a certified reference material. Microwave Assisted Solvent Extraction was compared to Soxhlet extraction.
{"title":"Clossed-vessel assisted microwave extraction of polychlorinated biphenyls in marine mussels","authors":"N. Carro, I. García, M. Llompart","doi":"10.1051/ANALUSIS:2000142","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000142","url":null,"abstract":"A reliable and simple procedure to extract polychlorinated biphenyls (PCBs) from marine mussels using microwave energy is proposed. Freeze-dried mussels were subjected to MASE (Microwave Assisted Solvent Extraction) in a closed-vessel microwave system with n-pentane-sodium hydroxide (5 %) or dichloromethane-pentane (1:1) at different temperatures (70 and 90 oC), the extraction time was 10 minutes. Sample extract cleanup procedure was performed by using alumina. Gas chromatog- raphy-mass spectrometry and gas chromatography-electron capture detector were employed for individual congener identification and determination. The influence of the following variables on microwave extraction of PCBs has been studied: extraction tem- perature, solvent volume, solvent nature, cleanup procedure time and volume of sodium hydroxide solution. Recoveries for PCBs were between 77 and 106 % with relative standard deviation between 2 to 20 %. Validation of the extraction process was carried out by processing a certified reference material. Microwave Assisted Solvent Extraction was compared to Soxhlet extraction.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"46 1","pages":"720-724"},"PeriodicalIF":0.0,"publicationDate":"2000-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74172483","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2000-10-01DOI: 10.1051/ANALUSIS:2000280686
A. García-Campaña, W. Baeyens
The potentials and possibilities offered by the rather unknown chemiluminescence-based analytical technique are discussed. Simplificity of instrumentation, low detection limits for various systems, and the inherent power of application to a vast number of natively fluorescing species or fluorophores formed after chemical derivatization broaden the scope of this relatively new detection technique. Drawbacks should be mentioned as well, amongst others limited selectiity of analysis (unless coupled to a powerful separational set-up), unexpected poor sensitivities for various analytes and the need to include an extra reaction step in the analytical procedures. Apart from the earlier gas-phase applications, the analysis in flowing streams (flow injection analysis, HPLC, and even capillary electrophoresis) has increased exponentially starting back in the early eighties. Various reagents have become available, including some originating from bioluminescent reactions (e.g. for ATP- and related analysis), not to forget the light emission as produced by diverse oxidation reactions, many of which the exact chemical pathways are not elucidated yet. On top of this, the power of chemiluminescence induction and measurements as applied to immunoassays, in the development of sensors, and, even more important, in the fast developing area of micromachining (sub-droplet-sized capillary electrophoresis) are discussed.
{"title":"Principles and recent analytical applications of chemiluminescence.","authors":"A. García-Campaña, W. Baeyens","doi":"10.1051/ANALUSIS:2000280686","DOIUrl":"https://doi.org/10.1051/ANALUSIS:2000280686","url":null,"abstract":"The potentials and possibilities offered by the rather unknown chemiluminescence-based analytical technique are discussed. Simplificity of instrumentation, low detection limits for various systems, and the inherent power of application to a vast number of natively fluorescing species or fluorophores formed after chemical derivatization broaden the scope of this relatively new detection technique. Drawbacks should be mentioned as well, amongst others limited selectiity of analysis (unless coupled to a powerful separational set-up), unexpected poor sensitivities for various analytes and the need to include an extra reaction step in the analytical procedures. Apart from the earlier gas-phase applications, the analysis in flowing streams (flow injection analysis, HPLC, and even capillary electrophoresis) has increased exponentially starting back in the early eighties. Various reagents have become available, including some originating from bioluminescent reactions (e.g. for ATP- and related analysis), not to forget the light emission as produced by diverse oxidation reactions, many of which the exact chemical pathways are not elucidated yet. On top of this, the power of chemiluminescence induction and measurements as applied to immunoassays, in the development of sensors, and, even more important, in the fast developing area of micromachining (sub-droplet-sized capillary electrophoresis) are discussed.","PeriodicalId":8221,"journal":{"name":"Analusis","volume":"64 1","pages":"686-698"},"PeriodicalIF":0.0,"publicationDate":"2000-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88923517","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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