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1.
Two new marine sediment standard reference materials (SRMs) for the determination of organic contaminants 总被引:3,自引:0,他引:3
Wise SA Poster DL Schantz MM Kucklick JR Sander LC Lopez de Alda M Schubert P Parris RM Porter BJ 《Analytical and bioanalytical chemistry》2004,378(5):1251-1264
Two new marine sediment standard reference materials (SRMs), SRM 1941b Organics in Marine Sediment and SRM 1944 New York/New Jersey Waterway Sediment, have been recently issued by the National Institute of Standards and Technology (NIST) for the determination of organic contaminants including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyl (PCB) congeners, and chlorinated pesticides. Both sediment SRMs were analyzed using multiple analytical methods including gas chromatography/mass spectrometry (GC/MS) on columns with different selectivity, reversed-phase liquid chromatography with fluorescence detection (for PAHs only), and GC with electron capture detection (for PCBs and pesticides only). SRM 1941b has certified concentrations for 24 PAHs, 29 PCB congeners, and 7 pesticides, and SRM 1944 has certified concentrations for 24 PAHs, 29 PCB congeners, and 4 pesticides. Reference concentrations are also provided for an additional 58 (SRM 1941b) and 39 (SRM 1944) PAHs, PCB congeners, and pesticides. SRM 1944, which was collected from multiple sites within New York/New Jersey coastal waterways, has contaminant concentrations that are generally a factor of 10–20 greater than SRM 1941b, which was collected in the Baltimore (Maryland) harbor. These two SRMs represent the most extensively characterized marine sediment certified reference materials available for the determination of organic contaminants.Electronic Supplementary Material Supplementary material is available in the online version of this article at . A link in the frame on the left on that page takes you directly to the supplementary material. 相似文献
2.
Stapleton HM Harner T Shoeib M Keller JM Schantz MM Leigh SD Wise SA 《Analytical and bioanalytical chemistry》2006,384(3):791-800
Polybrominated diphenyl ethers (PBDEs) have been measured for the first time in three different indoor dust Standard Reference
Materials (SRMs) prepared by the National Institute of Standards and Technology (NIST). Two of these, SRM 2583 (Trace Elements
in Indoor Dust) and SRM 2584 (Trace Elements in Indoor Dust), have been certified previously for lead and other inorganic
constituents. A third, SRM 2585 (Organics in Indoor Dust), is a new indoor dust reference material prepared by NIST which
will be certified for various organic compounds (polycyclic aromatic hydrocarbons, pesticides and polychlorinated biphenyls)
in 2005 including certified concentrations for 16 individual PBDE congeners and reference values for an additional three PBDE
congeners. Dust SRMs were analyzed for 30 PBDE congeners using high-resolution gas chromatography combined with low-resolution
mass spectrometry operated in both negative chemical ionization (GC/ECNI–MS) and electron impact ionization (GC/EI–MS) modes.
Sensitivity was an order of magnitude higher using GC/ECNI–MS relative to GC/EI–MS. These SRMs have been characterized and
compared to the three PBDE commercial products (pentaBDE, octaBDE and decaBDE). PentaBDE and DecaBDE were present in all three
SRMs and were the dominant commercial products, making up approximately 33% and 58%, respectively. Recent studies suggest
that house dust may be a leading source of human exposure to PBDEs. These SRMs are the first reference materials with certified
concentrations for PBDEs, which will aid in validating future measurements of PBDEs in house dust and other similar matrices.
Electronic Supplementary Material Supplementary material is available for this article at http://dx.doi.org/ 10.1007/s00216-005-0227-y 相似文献
3.
Wise SA Poster DL Kucklick JR Keller JM Vanderpol SS Sander LC Schantz MM 《Analytical and bioanalytical chemistry》2006,386(4):1153-1190
For the past 25 years the National Institute of Standards and Technology (NIST) has developed certified reference materials
(CRMs), known as standard reference materials (SRMs), for determination of organic contaminants in environmental matrices.
Assignment of certified concentrations has usually been based on combining results from two or more independent analytical
methods. The first-generation environmental-matrix SRMs were issued with certified concentrations for a limited number (5
to 10) of polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs). Improvements in the analytical certification
approach significantly expanded the number and classes of contaminants determined. Environmental-matrix SRMs currently available
include air and diesel particulate matter, coal tar, marine and river sediment, mussel tissue, fish oil and tissue, and human
serum, with concentrations typically assigned for 50 to 90 organic contaminants, for example PAHs, nitro-substituted PAHs,
PCBs, chlorinated pesticides, and polybrominated diphenyl ethers (PBDEs).
Electronic supplementary material Supplementary material is available in the online version of this article at and is accessible for authorized users. 相似文献
4.
Determination of polybrominated diphenyl ethers in marine biological tissues using microwave-assisted extraction 总被引:4,自引:0,他引:4
Growing concern on the environmental impact of polybrominated diphenyl ethers (PBDEs) has created the need for rapid and quality assured analytical methods to quantify PBDEs in a spectrum of matrix types. This study presents the first validated method for the quantification of major PBDE congeners (47, 99 and 100) in marine biological tissues using microwave-assisted extraction (MAE). The recovery of polychlorinated biphenyls and various organochlorine pesticides has also been ascertained. Analytical accuracy, precision, limits of detection and cleanup efficiency were evaluated for PBDE congeners, and empirical data justifies the use of MAE for the extraction and analysis of PBDEs in biological matrices. MAE was also compared to Soxhlet extraction efficiency for PBDEs in the standard reference materials SRM2978 and SRM1588a and gave comparable results (<15% variation). 相似文献
5.
Poster DL Schantz MM Kucklick JR Lopez de Alda MJ Porter BJ Pugh R Wise SA 《Analytical and bioanalytical chemistry》2004,378(5):1213-1231
Three new mussel tissue standard reference materials (SRMs) have been developed by the National Institute of Standards and Technology (NIST) for the determination of the concentrations of organic contaminants. The most recently prepared material, SRM 1974b, is a fresh frozen tissue homogenate prepared from mussels (Mytilus edulis) collected in Boston Harbor, Massachusetts. The other two materials, SRMs 2977 and 2978, are freeze-dried tissue homogenates prepared from mussels collected in Guanabara Bay, Brazil and Raritan Bay, New Jersey, respectively. All three new mussel tissue SRMs complement the current suite of marine natural-matrix SRMs available from NIST that are characterized for a wide range of contaminants (organic and inorganic). SRM 1974b has been developed to replace its predecessor SRM 1974a, Organics in Mussel Tissue, for which the supply is depleted. Similarly, SRMs 2977 and 2978 were developed to replace a previously available (supply depleted) freeze-dried version of SRM 1974a, SRM 2974, Organics in Freeze-Dried Mussel Tissue. SRM 1974b is the third in a series of fresh frozen mussel tissue homogenate SRMs prepared from mussels collected in Boston Harbor starting in 1988. SRM 1974b has certified concentration values for 22 polycyclic aromatic hydrocarbons (PAHs), 31 polychlorinated biphenyl congeners (PCBs), and 7 chlorinated pesticides. Reference values are provided for additional constituents: 16 PAHs, 8 PCBs plus total PCBs, 6 pesticides, total extractable organics, methylmercury, and 11 trace elements. PAH concentrations range from about 2 ng g–1 dry mass (cyclopenta[cd]pyrene) to 180 ng g–1 dry mass (pyrene). PCB concentrations range from about 2 ng g–1 dry mass (PCB 157) to 120 ng g–1 dry mass (PCB 153). The reference value for total PCBs in SRM 1974b is (2020 ± 420) ng g–1 dry mass. Pesticide concentrations range from about 4 ng g–1 dry mass (4,4-DDT) to 40 ng g–1 dry mass (4,4-DDE). SRM 2977 has certified values for 14 PAHs, 25 PCB congeners, 7 pesticides, 6 trace elements, and methylmercury. Reference values for 16 additional PAHs and 9 inorganic constituents are provided, and information values are given for 23 additional trace elements. SRM 2978 has certified and reference concentrations for 41 and 22 organic compounds, respectively, and contains contaminant levels similar to those of SRM 1974b. Organic contaminant levels in SRM 2977 (mussels from Guanabara Bay, Brazil) are typically a factor of 2 to 4 lower than those in SRM 1974b and SRM 2978. The organic contaminant concentrations in each new mussel tissue SRM are presented and compared in this paper. In addition, a chronological review of contaminant concentrations associated with mussels collected in Boston Harbor is discussed as well as a stability assessment of SRM 1974a.Electronic Supplementary Material Supplementary material is available in the online version of this article at . A link in the frame on the left on that page takes you directly to the supplementary material. 相似文献
6.
John R. Kucklick Michele M. Schantz Rebecca S. Pugh Barbara J. Porter Dianne L. Poster Paul R. Becker Teri K. Rowles Stefan Leigh Stephen A. Wise 《Analytical and bioanalytical chemistry》2010,397(2):423-432
The National Institute of Standards and Technology (NIST) has a diverse collection of control materials derived from marine
mammal blubber, fat, and serum. Standard Reference Material (SRM) 1945 Organics in Whale Blubber was recertified for polychlorinated
biphenyl (PCB) congeners, organochlorine pesticides, and polybrominated diphenyl ether (PBDE) congeners. SRM 1945 has also
been assigned mass fraction values for compounds not frequently determined in marine samples including toxaphene congeners,
coplanar PCBs, and methoxylated PBDE congeners which are natural products. NIST also has assigned mass fraction values, as
a result of interlaboratory comparison exercises, for PCB congeners, organochlorine pesticides, PBDE congeners, and fatty
acids in six homogenate materials produced from marine mammal blubber or serum. The materials are available from NIST upon
request; however, the supply is very limited for some of the materials. The materials include those obtained from pilot whale
blubber (Homogenates III and IV), Blainville’s beaked whale blubber (Homogenate VII), polar bear fat (Homogenate VI), and
California sea lion serum (Marine Mammal Control Material-1 Serum) and blubber (Homogenate V). 相似文献
7.
Poster DL Kucklick JR Schantz MM Porter BJ Leigh SD Wise SA 《Analytical and bioanalytical chemistry》2003,375(2):223-241
The concentrations of a wide range of polychlorinated biphenyl congeners (PCBs) and chlorinated pesticides in a fish tissue Standard Reference Material (SRM) have been determined using multiple methods of analysis. This material, SRM 1946, Lake Superior Fish Tissue, was recently issued by the National Institute of Standards and Technology (NIST) and complements a suite of marine environmental natural-matrix SRMs that are currently available from NIST for the determination of organic contaminants such as aliphatic hydrocarbons, polycyclic aromatic hydrocarbons (PAHs), PCBs, and chlorinated pesticides. SRM 1946 is a fresh tissue homogenate (frozen) prepared from filleted adult lake trout (Salvelinus namaycush namaycush) collected from the Apostle Islands region of Lake Superior. SRM 1946 has certified and reference concentrations for PCB congeners, including the three non- ortho PCB congeners, and chlorinated pesticides. Certified concentrations are available for 30 PCB congeners and 15 chlorinated pesticides. Reference concentrations are available for 12 PCB congeners and 2 chlorinated pesticides. In addition, SRM 1946 is characterized for additional chemical constituents and properties: fatty acids, extractable fat, methylmercury, total mercury, selected trace elements, proximates, and caloric content. The characterization of chlorinated compounds is described in this paper with an emphasis on the approach used for the certification of the concentrations of PCB congeners and chlorinated pesticides. The PCB congener and chlorinated pesticide data are also compared to concentrations in other marine natural-matrix reference materials available from NIST (fish oil, mussel tissue, whale blubber, and a second fresh frozen fish tissue homogenate prepared from filleted adult lake trout collected from Lake Michigan) and from other organizations such as the National Research Council Canada (ground whole carp), the International Atomic Energy Agency (fish homogenate), and the European Commission Joint Research Centre [fish oils (cod and mackerel) and mussel tissue]. 相似文献
8.
Schantz MM Keller JM Leigh S Patterson DG Sharpless KE Sjödin A Stapleton HM Swarthout R Turner WE Wise SA 《Analytical and bioanalytical chemistry》2007,389(4):1201-1208
The Certificate of Analysis for SRM 1589a PCBs, Pesticides, PBDEs, and Dioxins/Furans in Human Serum has been updated to include
certified concentration values for 27 polychlorinated biphenyl (PCB) congeners, three chlorinated pesticides, and four polybrominated
diphenyl ether (PBDE) congeners as well as reference concentration values for 27 additional PCB congeners, six additional
chlorinated pesticides, three additional PBDE congeners, and selected polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs). This represents an addition of concentration values for 29 PCB
congeners and for PBDE congeners that were not quantified in the previous issue of SRM 1589a. With the increased number of
certified and reference concentration values for PCBs and the inclusion of certified and reference concentration values for
PBDEs, this serum material will be more useful as a reference material for contaminant monitoring in human tissues and fluids.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
9.
Kucklick JR Tuerk KJ Vander Pol SS Schantz MM Wise SA 《Analytical and bioanalytical chemistry》2004,378(5):1147-1151
Polybrominated diphenyl ether (PBDE) congeners and components of the complex mixture toxaphene are stable in the environment and readily bioaccumulated into wildlife and human tissues. PBDEs are presently used in large quantities worldwide as flame retardants in textiles, furniture, computer equipment, and cables. Toxaphene is a complex mixture of chlorinated bornanes and bornenes that was the most heavily used pesticide in the United States until it was banned in 1982; however, some countries continue to use toxaphene. The National Institute of Standards and Technology has quantified PBDE congeners and toxaphene in several available Standard Reference Materials (SRMs) using methods of gas chromatography with electron impact mass spectrometry (GC-EI-MS) and GC negative chemical ionization (NCI) MS, respectively. SRM 1588a Organics in Cod Liver Oil and SRM 1945 Organics in Whale Blubber were examined for PBDE congeners 47, 99, 100, 153, and 154, total toxaphene, and toxaphene congeners 26, 50, and 62. SRM 1946 Lake Superior Fish Tissue was also examined for total toxaphene and toxaphene congeners. The sum of the PBDE congeners (mean, (1 SD) wet basis) for SRM 1945 was 150 ng g–1 (7 ng g–1). The concentration of PBDE 47 in SRM 1588a was 82.7 ng g–1 (2.8 ng g–1). Other PBDEs were detected in SRM 1588a but were not quantified due their low levels. The total toxaphene (wet mass basis) was 1,210 ng g–1 (127 ng g–1), 1,960 ng g–1 (133 ng g–1), and 3,980 ng g–1 (248 ng g–1) in SRMs 1945, 1946, and 1588a, respectively. The values for PBDEs and toxaphene determined in the SRMs, while not certified, indicate that the SRMs will be suitable control materials for PBDE and toxaphene analyses. 相似文献
10.
Davis WC Christopher SJ Pugh RS Donard OF Krupp EA Point D Horvat M Gibicar D Kljakovic-Gaspic Z Porter BJ Schantz MM 《Analytical and bioanalytical chemistry》2007,387(7):2335-2341
This paper describes the development of two independent analytical methods for the extraction and quantification of methylmercury
from marine biota. The procedures involve microwave extraction, followed by derivatization and either headspace solid-phase
microextraction (SPME) with a polydimethylsiloxane (PDMS)-coated silica fiber or back-extraction into iso-octane. The identification
and quantification of the extracted compounds is carried out by capillary gas chromatography/mass spectrometric (GC/MS) and
inductively coupled plasma mass spectrometric (GC/ICP-MS) detection. Both methods were validated for the determination of
methylmercury (MeHg) concentrations in a variety of biological standard reference materials (SRMs) including fresh-frozen
tissue homogenates of SRM 1946 Lake Superior fish tissue and SRM 1974a organics in mussel tissue (Mytilus edulis) and then applied to the certification effort of SRM 1947 Lake Michigan fish tissue and SRM 1974b organics in mussel tissue
(Mytilus edulis). While past certifications of methylmercury in tissue SRMs have been based on two independent methods from the National
Institute of Standards and Technology (NIST) and participating laboratories, the methods described within provide improved
protocols and will allow future certification efforts to be based on at least two independent analytical methods within NIST. 相似文献
11.
Point D Davis WC Christopher SJ Ellisor MB Pugh RS Becker PR Donard OF Porter BJ Wise SA 《Analytical and bioanalytical chemistry》2007,387(7):2343-2355
An accurate, ultra-sensitive and robust method for speciation of mono, di, and tributyltin (MBT, DBT, and TBT) by speciated isotope-dilution gas chromatography-inductively coupled plasma-mass spectrometry (SID-GC-ICPMS) has been developed for quantification of butyltin concentrations in cryogenic biological materials maintained in an uninterrupted cryo-chain from storage conditions through homogenization and bottling. The method significantly reduces the detection limits, to the low pg g(-1) level (as Sn), and was validated by using the European reference material (ERM) CE477, mussel tissue, produced by the Institute for Reference Materials and Measurements. It was applied to three different cryogenic biological materials-a fresh-frozen mussel tissue (SRM 1974b) together with complex materials, a protein-rich material (whale liver control material, QC03LH03), and a lipid-rich material (whale blubber, SRM 1945) containing up to 72% lipids. The commutability between frozen and freeze-dried materials with regard to spike equilibration/interaction, extraction efficiency, and the absence of detectable transformations was carefully investigated by applying complementary methods and by varying extraction conditions and spiking strategies. The inter-method results enabled assignment of reference concentrations of butyltins in cryogenic SRMs and control materials for the first time. The reference concentrations of MBT, DBT, and TBT in SRM 1974b were 0.92 +/- 0.06, 2.7 +/- 0.4, and 6.58 +/- 0.19 ng g(-1) as Sn (wet-mass), respectively; in SRM 1945 they were 0.38 +/- 0.06, 1.19 +/- 0.26, and 3.55 +/- 0.44 ng g(-1), respectively, as Sn (wet-mass). In QC03LH03, DBT and TBT concentrations were 30.0 +/- 2.7 and 2.26 +/- 0.38 ng g(-1) as Sn (wet-mass). The concentration range of butyltins in these materials is one to three orders of magnitude lower than in ERM CE477. This study demonstrated that cryogenically processed and stored biological materials are a promising alternative to conventional freeze-dried materials for organotin speciation analysis, because these are, at present, the best conditions for minimizing degradation of thermolabile species and for long-term archival. Finally, the potential of the analytical method was illustrated by analysis of polar bear (Ursus maritimus) and beluga whale (Delphinapterus leuca) liver samples that had been collected in the Arctic and archived at the Marine Environmental Specimen Bank. Significant concentrations of butyltin compounds were found in the samples and provide the first evidence of the presence of this class of contaminant in the Arctic marine ecosystem. Figure Eye catch image. 相似文献
12.
Deena M. Butryn Michael S. Gross Lai-Har Chi Arnold Schecter James R. Olson Diana S. Aga 《Analytica chimica acta》2015
The presence of polybrominated diphenyl ethers (PBDEs) and their hydroxylated (OH-BDE) and methoxylated (MeO-BDE) analogs in humans is an area of high interest to scientists and the public due to their neurotoxic and endocrine disrupting effects. Consequently, there is a rise in the investigation of the occurrence of these three classes of compounds together in environmental matrices and in humans in order to understand their bioaccumulation patterns. Analysis of PBDEs, OH-BDEs, and MeO-BDEs using liquid chromatography-mass spectrometry (LC-MS) can be accomplished simultaneously, but detection limits for PBDEs and MeO-BDEs in LC-MS is insufficient for trace level quantification. Therefore, fractionation steps of the phenolic (OH-BDEs) and neutral (PBDEs and MeO-BDEs) compounds during sample preparation are typically performed so that different analytical techniques can be used to achieve the needed sensitivities. However, this approach involves multiple injections, ultimately increasing analysis time. In this study, an analytical method was developed for a “one-shot” analysis of 12 PBDEs, 12 OH-BDEs, and 13 MeO-BDEs using gas chromatography with tandem mass spectrometry (GC-MS/MS). This overall method includes simultaneous extraction of all analytes via pressurized liquid extraction followed by lipid removal steps to reduce matrix interferences. The OH-BDEs were derivatized using N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide (TBDMS-MTFA), producing OH-TBDMS derivatives that can be analyzed together with PBDEs and MeO-BDEs by GC-MS/MS in “one shot” within a 25-min run time. The overall recoveries were generally higher than 65%, and the limits of detection ranged from 2 to 14 pg in both breast milk and serum matrices. The applicability of the method was successfully validated on four paired human breast milk and serum samples. The mean concentrations of total PBDEs, OH-BDEs, and MeO-BDEs in breast milk were 59, 2.2, and 0.57 ng g−1 lipid, respectively. In serum, the mean total concentrations were 79, 38, and 0.96 ng g−1 lipid, respectively, exhibiting different distribution profiles from the levels detected in breast milk. This “one-shot” GC-MS/MS method will prove useful and cost-effective in large-scale studies needed to further understand the partitioning behavior, and ultimately the adverse health effects, of these important classes of brominated flame retardants in humans. 相似文献
13.
Frank C. Calvosa 《Talanta》2010,80(3):1116-6727
The extraction of polybrominated diphenyl ethers (PBDEs) from SRM 2585 (Organic Contaminants in House Dust) was investigated using supercritical fluid R134a as an extraction solvent. Three methods of dust extraction were studied: (1) extraction of dry dust, (2) extraction of dry dust dispersed on Ottawa sand and (3) extraction of dust wet with dichloromethane. For each of the three sample preparation methods, extracts at three temperatures (110, 150, and 200 °C) above the critical temperature of R134a were performed. Eight PBDE congeners (BDE-28, -47, -99, 100, -153, -154, -183, and -209) in the SFE extracts were analyzed by liquid chromatography negative-ion atmospheric pressure photoionization tandem mass spectrometry (LC/NI-APPI/MS/MS). The optimum extraction of PBDEs from house dust using supercritical R134a is obtained when the dust is pre-wet with dichloromethane prior to extraction to swell the dust. For all sample preparation methods, higher temperatures afforded higher percent recoveries of the eight PBDE congeners. Only a combination of high-temperature (200 °C) and pre-wetting the dust with dichloromethane produced high recovery of the environmentally important, fully brominated PBDE congener, BDE-209. 相似文献
14.
Determination of polybrominated diphenyl ethers in freshwater fishes from a river polluted by e-wastes 总被引:4,自引:0,他引:4
Analytical method using mass spectrometric techniques was applied for the determination of polybrominated diphenyl ethers (PBDEs) in freshwater fishes. Fish samples collected from Nanyang River contaminated by the recycling electron-wastes (e-wastes) materials were prepared by using Soxhlet extraction and multiple-step column chromatographic clean-up. PBDEs were determined by gas chromatography (GC) coupled with ion trap mass spectrometry (for mono- to hepta-BDEs) and quadrupole mass spectrometry (for BDE-209). The method performance was evaluated with the recovery of 13C-labeled internal standards and with the analysis of certified reference biota. The obtained recoveries ranged from 75 to 125% with a relative standard deviation of lower than 10% for 16 PBDE congeners. The total PBDE (ΣPBDE) concentrations in fishes showed the following trend: grass carp < mud carp < crucian carp < silver carp < carp. ΣPBDE concentrations in the abdomen, back and tail muscles of carp ranged from 766, 458 and 530 ng/g w.w., and 53, 52, 45 ng/g w.w. in grass carp, respectively. The ΣPBDE concentrations in abdomen muscles were no significantly higher than in back and tail muscles in carp, crucian carp, grass carp and mud carp. PBDE congener concentrations in muscles correlated well with their lipid content. BDE-47 and BDE-28 were the most abundant congeners followed by BDE-17, BDE-15, BDE-66, BDE-154 and BDE-153 in fishes collected from Guiyu. 相似文献
15.
Stephen A. Wise Michele M. Schantz Bruce A. Benner Jr. Reenie M. Parris Richard E. Rebbert Lane C. Sander Barbara J. Koster Stephen N. Chesler Willie E. May 《Fresenius' Journal of Analytical Chemistry》1993,345(2-4):325-329
Summary Recent activities at the National Institute of Standards and Technology (NIST) related to the development of standard reference materials (SRMs) for the determination of polycyclic aromatic hydrocarbons (PAHs) are described. These activities include: (1) the development of four new calibration solution SRMs, a marine sediment SRM, and a frozen mussel tissue SRM; (2) noncertified measurements of PAHs for two additional sediment SRMs; and (3) the establishment of reference Ames bioassay mutagenicity values on three existing SRMs. Activities in progress include the recertification of the existing air particulate and diesel particulate SRMs and the preparation of a new diesel particulate extract SRM. 相似文献
16.
Akifumi Eguchi Tomohiko Isobe Karri Ramu 《International journal of environmental analytical chemistry》2013,93(4):348-356
An analytical method for higher brominated congeners of polybrominated diphenyl ethers (PBDEs) was optimised using a gas chromatograph equipped with an electron impact ionisation-quadrupole mass spectrometer (GC-EI-qMS) and five native PBDEs and three 13C12-labelled congeners in biological and environmental samples (mussels, sediment, dust). In the optimised instrumental conditions, abundance and repeatability improved with increase in temperature of the ion source. The instrumental detection limits (IDLs) for BDE-196, BDE-197, BDE-206, BDE-207 and BDE-209 were 0.1, 0.1, 0.2, 0.3 and 0.6?pg, respectively. When compared to the previous reports, the IDLs were the same as for electron capture negative ionisation (ECNI) or EI-double focusing magnetic sector (EI-Sector) mass spectrometer, indicating that sensitive determination could be achieved using a conventional GC-EI-qMS. Validation of the method was carried out by the analysis of reference materials and mussel samples. We confirmed that the concentrations quantified using this method was in the range of reported values for reference materials. Similar concentrations were found in mussels, which were analysed previously by our group. Thus, we conclude that a conventional GC-EI-qMS can be applied for analysis of higher brominated PBDEs in various environmental and biota matrices. 相似文献
17.
Determination of perfluorinated alkyl acid concentrations in biological standard reference materials
Jessica L. Reiner Steven G. O’Connell Craig M. Butt Scott A. Mabury Jeff M. Small Amila O. De Silva Derek C. G. Muir Amy D. Delinsky Mark J. Strynar Andrew B. Lindstrom William K. Reagen Michelle Malinsky Sandra Sch?fer Christiaan J. A. F. Kwadijk Michele M. Schantz Jennifer M. Keller 《Analytical and bioanalytical chemistry》2012,404(9):2683-2692
Standard reference materials (SRMs) are homogeneous, well-characterized materials used to validate measurements and improve the quality of analytical data. The National Institute of Standards and Technology (NIST) has a wide range of SRMs that have mass fraction values assigned for legacy pollutants. These SRMs can also serve as test materials for method development, method validation, and measurement for contaminants of emerging concern. Because inter-laboratory comparison studies have revealed substantial variability of measurements of perfluoroalkyl acids (PFAAs), future analytical measurements will benefit from determination of consensus values for PFAAs in SRMs to provide a means to demonstrate method-specific performance. To that end, NIST, in collaboration with other groups, has been measuring concentrations of PFAAs in a variety of SRMs. Here we report levels of PFAAs and perfluorooctane sulfonamide (PFOSA) determined in four biological SRMs: fish tissue (SRM 1946 Lake Superior Fish Tissue, SRM 1947 Lake Michigan Fish Tissue), bovine liver (SRM 1577c), and mussel tissue (SRM 2974a). We also report concentrations for three in-house quality-control materials: beluga whale liver, pygmy sperm whale liver, and white-sided dolphin liver. Measurements in SRMs show an array of PFAAs, with perfluorooctane sulfonate (PFOS) being the most frequently detected. Reference and information values are reported for PFAAs measured in these biological SRMs. Figure
NIST SRMs 1946 Lake Superior Fish Tissue and 1947 Lake Michigan Fish Tissue 相似文献
18.
This study presents a time‐ and solvent‐saving method, pressurized liquid extraction (PLE), to extract polybrominated diphenyl ethers (PBDEs) in sediment samples. The effects of various operating parameters (i.e., extraction solution, temperature, pressure, static/dynamic extraction times) for the quantitative extraction of PBDEs by home‐made PLE were systematically investigated and optimized. The analytes were then identified and quantitated by gas chromatography‐mass spectrometry (GC‐MS) in selected ion monitoring (SIM) mode. The 16 PBDE congeners (from tri‐ to deca‐BDE) can be completely extracted by dichloromethane: n‐hexane (3/2, v/v) at 100 °C and 100 atm combined with 15 min static and then 15 min dynamic extraction steps. Recovery of PBDEs in spiked sediment samples ranged from 52 to 104% with 2‐16% RSD, except for BDE‐206. Limits of quantitation (LOQ) were established between 4 and 400 pg/g (dry weight) in 10 g of sediment sample. The extraction efficiency of the PLE was also compared with the traditional Soxhlet extraction method. The total contents of PBDEs ranged from 8.0 to 37.9 ng/g (dry weight) in various river and coastal sediment samples in Taiwan. Deca‐BDE (BDE‐209) was the major PBDE detected in these sediment samples. 相似文献
19.
20.
Instrumental methods and challenges in quantifying polybrominated diphenyl ethers in environmental extracts: a review 总被引:1,自引:0,他引:1
Stapleton HM 《Analytical and bioanalytical chemistry》2006,386(4):807-817
Increased interest in the fate, transport and toxicity of polybrominated diphenyl ethers (PBDEs) over the past few years has
led to a variety of studies reporting different methods of analysis for these persistent organic pollutants. Because PBDEs
encompass a range of vapor pressures, molecular weights and degrees of bromine substitution, various analytical methods can
lead to discrimination of some PBDE congeners. Recent improvements in injection techniques and mass spectrometer ionization
methods have led to a variety of options to determine PBDEs in environmental samples. The purpose of this paper is therefore
to review the available literature describing the advantages and disadvantages in choosing an injection technique, gas chromatography
column and detector. Additional discussion is given to the challenges in measuring PBDEs, including potential chromatographic
interferences and the lack of commercial standards for higher brominated congeners, which provides difficulties in examining
degradation and debromination of BDE congeners, particularly for BDE 209. 相似文献