Three new mussel tissue standard reference materials (SRMs) for the determination of organic contaminants

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.     

Two new marine sediment standard reference materials (SRMs) for the determination of organic contaminants

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.     

Marine mammal blubber reference and control materials for use in the determination of halogenated organic compounds and fatty acids

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).     

Certification of methylmercury content in two fresh-frozen reference materials: SRM 1947 Lake Michigan fish tissue and SRM 1974b organics in mussel tissue (Mytilus edulis)

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.     

Certification of standard reference material (SRM) 1941a, organics in marine sediment

SRM 1941a, Organics in Marine Sediment, has been recently issued with certified concentrations for 23 polycyclic aromatic hydrocarbons, 21 polychlorinated biphenyl congeners, 6 chlorinated pesticides, and sulfur. Noncertified concentrations have been also reported for additional PAHs, PCB congeners, and chlorinated pesticides and for percent total organic carbon (TOC), aliphatic hydrocarbons, and trace elements. SRM 1941a is the most extensively characterized natural matrix SRM issued by the National Institute of Standards and Technology (NIST).     

Analysis of urban particulate standard reference materials for the determination of chlorinated organic contaminants and additional chemical and physical properties

A previously issued National Institute of Standards and Technology (NIST) Standard Reference Material (SRM), SRM 1649, Urban Dust/Organics has been analyzed for chlorinated organic contaminants (polychlorinated biphenyls and chlorinated pesticides) to provide certified values for a new class of compounds relative to the former certification. The material will be reissued as SRM 1649a. Four different analytical techniques were used. Specifically, two different methods of extraction (Soxhlet and pressurized fluid extraction) were used in conjunction with sample analysis by gas chromatography with two different columns (5% phenyl-methyl polysiloxane and 50% methyl C-18 dimethyl polysiloxane) that exhibit distinct selectivity, and with two different modes of detection (electron capture detection and mass spectrometry). The results from these techniques were combined to generate certified concentrations for 35 PCB congeners (some in combination) and 8 chlorinated pesticides. Ancillary assessments of additional chemical and physical properties of SRM 1649a include homogeneity, moisture, total organic carbon, extractable mass, and the particle-size distribution. The approach and the results for the certification of the PCB congeners and chlorinated pesticides in SRM 1649a, and the determination of the additional chemical and physical properties are described. In addition, the determination of PCBs and chlorinated pesticides in SRM 1648, Urban Particulate Matter (a particulate material certified for inorganic constituents), is also discussed although certified values are not presented. Received: 8 June 1998 / Revised: 4 September 1998 / Accepted: 26 September 1998     

Analysis of urban particulate standard reference materials for the determination of chlorinated organic contaminants and additional chemical and physical properties

A previously issued National Institute of Standards and Technology (NIST) Standard Reference Material (SRM), SRM 1649, Urban Dust/Organics has been analyzed for chlorinated organic contaminants (polychlorinated biphenyls and chlorinated pesticides) to provide certified values for a new class of compounds relative to the former certification. The material will be reissued as SRM 1649a. Four different analytical techniques were used. Specifically, two different methods of extraction (Soxhlet and pressurized fluid extraction) were used in conjunction with sample analysis by gas chromatography with two different columns (5% phenyl-methyl polysiloxane and 50% methyl C-18 dimethyl polysiloxane) that exhibit distinct selectivity, and with two different modes of detection (electron capture detection and mass spectrometry). The results from these techniques were combined to generate certified concentrations for 35 PCB congeners (some in combination) and 8 chlorinated pesticides. Ancillary assessments of additional chemical and physical properties of SRM 1649a include homogeneity, moisture, total organic carbon, extractable mass, and the particle-size distribution. The approach and the results for the certification of the PCB congeners and chlorinated pesticides in SRM 1649a, and the determination of the additional chemical and physical properties are described. In addition, the determination of PCBs and chlorinated pesticides in SRM 1648, Urban Particulate Matter (a particulate material certified for inorganic constituents), is also discussed although certified values are not presented. Received: 8 June 1998 / Revised: 4 September 1998 / Accepted: 26 September 1998     

Comparison of methods for the gas-chromatographic determination of PCB congeners and chlorinated pesticides in marine reference materials

Summary Three gas-chromatographic (GC) columns with different selectivity (DB-5, DB-1701, and C-18) and two different GC detectors (electron-capture and mass-spectrometric) were used to analyze three Standard Reference Materials (SRMs), which are available from the National Institute of Standards and Technology (NIST), and two Certified Reference Materials (CRMs), which are available from the Community Bureau of Reference (BCR), for polychlorinated biphenyl (PCB) congeners and chlorinated pesticides. The materials analyzed were: SRM 1588, Organics in Cod Liver Oil; SRM 1941, Organics in Marine Sediment; SRM 1974, Organics in Mussel Tissue (Mytilus edulis); CRM 349, Chlorobiphenyls in Cod Liver Oil; and CRM 350, Chlorobiphenyls in Mackerel Oil. Results from these different methods are compared, and concentrations for additional PCB congeners and chlorinated pesticides in these reference materials, which have not been measured previously, are reported.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday     

Determination of perfluorinated alkyl acid concentrations in biological standard reference materials

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.

Certification of SRM 1589a PCBs,pesticides, PBDEs,and dioxins/furans in human serum

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.     

Synthetic musk fragrances in environmental Standard Reference Materials

Synthetic musk fragrances have been measured in water, air, sediments, sewage sludge, and biota worldwide. As the study of the environmental fate and impacts of these compounds progresses, the need for Standard Reference Materials (SRMs) for these compounds to facilitate analytical method improvement and interlaboratory comparisons becomes increasingly important. The National Institute of Standards and Technology (NIST) issues environmental matrix SRMs with certified concentrations for a variety of persistent organic pollutants including polycyclic aromatic hydrocarbons (PAHs), chlorinated pesticides, and polychlorinated biphenyl congeners (PCBs). Until now synthetic musk fragrance concentrations have not been reported in NIST SRMs. The objective of this study was to provide reference values for several commonly detected synthetic musk fragrances in several NIST natural matrix SRMs. In this study five polycyclic musk fragrances [HHCB (1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta-γ-2-benzopyran), AHTN (7-acetyl-1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydronaphthalene), ADBI (4-acetyl-1,1-dimethyl-6-tert-butylindane), AHMI (6-acetyl-1,1,2,3,3,5-hexamethylindane), and ATII (5-acetyl-1,1,2,6-tetramethyl-3-isopropylindane] and two nitro musk fragrances [musk xylene (1-tert-butyl-3,5-dimethyl-2,4,6-trinitrobenzene) and musk ketone (4-tert-butyl-3,5-dinitro-2,6-dimethylacetophenone)] were measured in selected environmental SRMs. Gas chromatography–electron impact mass spectrometry (GC/EI-MS) was used for all analyses. HHCB was the most frequently detected synthetic musk fragrance and was detected in SRM 2585 Organic Contaminants in House Dust, SRM 2781 Domestic Sludge, SRM 1974b Organics in Mussel Tissue (Mytilus edulis), and SRM 1947 Lake Michigan Fish Tissue. It was not detected in SRM 1946 Lake Superior Fish Tissue or SRM 1945 Organics in Whale Blubber. Concentrations of HHCB in these SRMs ranged from 1.12 ng/g in SRM 1947 to 92,901 ng/g in SRM 2781. All of the polycyclic musk fragrances were detected in SRM 2781 and all of the target compounds were detected in SRM 2585. Electronic supplementary material Supplementary material is available for this article at and is accessible to authorized users.     

Determination of polybrominated diphenyl ethers in environmental standard reference materials

Standard reference materials (SRMs) are valuable tools in developing and validating analytical methods to improve quality assurance standards. The National Institute of Standards and Technology (NIST) has a long history of providing environmental SRMs with certified concentrations of organic and inorganic contaminants. Here we report on new certified and reference concentrations for 27 polybrominated diphenyl ether (PBDE) congeners in seven different SRMs: cod-liver oil, whale blubber, fish tissue (two materials), mussel tissue and sediment (two materials). PBDEs were measured in these SRMs, with the lowest concentrations measured in mussel tissue (SRM 1974b) and the highest in sediment collected from the New York/New Jersey Waterway (SRM 1944). Comparing the relative PBDE congener concentrations within the samples, we found the biota SRMs contained primarily tetrabrominated and pentabrominated diphenyl ethers, whereas the sediment SRMs contained primarily decabromodiphenyl ether (BDE 209). The cod-liver oil (SRM 1588b) and whale blubber (SRM 1945) materials were also found to contain measurable concentrations of two methoxylated PBDEs (MeO-BDEs). Certified and reference concentrations are reported for 12 PBDE congeners measured in the biota SRMs and reference values are available for two MeO-BDEs. Results from a sediment interlaboratory comparison PBDE exercise are available for the two sediment SRMs (1941b and 1944).     

Standard reference materials (SRMs) for determination of organic contaminants in environmental samples

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.     

Determination of non-ortho polychlorinated biphenyls in environmental Standard Reference Materials

The concentrations of three non-ortho ("coplanar") polychlorinated biphenyls, 3,3',4,4'-tetrachlorobiphenyl (IUPAC PCB 77), 3,3',4,4',5-pentachlorobiphenyl (IUPAC PCB 126), and 3,3',4,4',5,5'-hexachlorobiphenyl (IUPAC PCB 169), were determined in five NIST Standard Reference Materials (SRMs) of environmental and biological interest. The measured levels were approximately between (0.2 to 1.3) ng/g in SRM 1588a (Organics in Cod Liver Oil), (0.3 to 9) ng/g in SRM 1944 (New York/New Jersey Waterway Sediment), (0.2 to 0.4) ng/g in SRM 1945 (Organics in Whale Blubber), (1 to 18) ng/g in SRM 2974 (Organics in Freeze-dried Mussel Tissue [Mytilus edulis]), and (0.1 to 0.4) ng/g in candidate SRM 1946 (Lake Superior Fish Tissue). PCB 169 was present at < 0.1 ng/g in SRMs 1944 and 2974.     

Determination of non-ortho polychlorinated biphenyls in environmental Standard Reference Materials

The concentrations of three non-ortho (“coplanar”) polychlorinated biphenyls, 3,3′,4,4′-tetrachlorobiphenyl (IUPAC PCB 77), 3,3′,4,4′,5-pentachlorobiphenyl (IUPAC PCB 126), and 3,3′,4,4′,5,5′-hexachlorobiphenyl (IUPAC PCB 169), were determined in five NIST Standard Reference Materials (SRMs) of environmental and biological interest. The measured levels were approximately between (0.2 to 1.3) ng/g in SRM 1588?a (Organics in Cod Liver Oil), (0.3 to 9) ng/g in SRM 1944 (New York/New Jersey Waterway Sediment), (0.2 to 0.4) ng/g in SRM 1945 (Organics in Whale Blubber), ¶(1 to 18) ng/g in SRM 2974 (Organics in Freeze-dried Mussel Tissue [Mytilus edulis]), and (0.1 to 0.4) ng/g ¶in candidate SRM 1946 (Lake Superior Fish Tissue). PCB 169 was present at < 0.1 ng/g in SRMs 1944 and 2974.     

Development of a murre (<Emphasis Type="Italic">Uria</Emphasis> spp.) egg control material

The Seabird Tissue Archival and Monitoring Project (STAMP) is a collaborative Alaska-wide effort by the US Fish and Wildlife Service’s Alaska Maritime National Wildlife Refuge (USFWS/AMNWR), the US Geological Survey’s Biological Resources Division (USGS/BRD), the Bureau of Indian Affairs Alaska Region Subsistence Branch (BIA/ARSB), and the National Institute of Standards and Technology (NIST) to monitor long-term (decadal) trends in environmental contaminants using seabird eggs. To support this effort, a matrix- (seabird egg) and concentration-specific control material was needed to ensure quality during analytical work. Although a herring gull egg quality assurance (HGQA) material is available from Environment Canada (EC), contaminant concentrations in this material tended to be higher than those observed in Alaskan murre (Uria spp.) eggs. Therefore, to prepare a more appropriate control material, a total of 12 common murre (U. aalge) and thick-billed murre (U. lomvia) eggs from four Bering Sea and Gulf of Alaska nesting locations were cryohomogenized to create 190 aliquots each containing approximately 6 g. This new control material was analyzed by different methods at NIST and EC facilities for the determination of concentrations and value assignment of 63 polychlorinated biphenyl (PCB) congeners, 20 organochlorine pesticides, and 11 polybrominated diphenyl ether (PBDE) congeners. The total PCB concentration is approximately 58 ng g⁻¹ wet mass. Results obtained for analytes not listed on the certificates of analysis of the previously used control materials, HGQA and NIST’s Standard Reference Material (SRM) 1946 Lake Superior Fish Tissue, are also presented.      

Preparation and analysis of a river sediment Standard Reference Material for the determination of trace organic constituents

Summary A river sediment Standard Reference Material (SRM) has been prepared and analyzed for determination of the concentrations of trace organic constituents. SRM 1939, Polychlorinated Biphenyls (PCBs) in River Sediment A, has been certified for the concentrations of three PCB congeners using the results obtained from capillary column gas chromatography with electron capture detection (GC-ECD) and from multidimensional (dual column) capillary gas chromatography with mass spectrometric detection (MCGC-MSD). For SRM certification, two independent analytical procedures are usually required. If only one analytical technique is used or if the procedures are not independent, then the concentrations are reported as noncertified or informational values rather than certified values. Noncertified values for 14 additional PCB congeners and five chlorinated pesticides, determined by GC-ECD, are also reported as well as noncertified concentrations for five polycyclic aromatic hydrocarbons (PAHs), determined using gas chromatography with mass spectrometric detection (GC-MSD). SRM 1939 complements SRM 1941, Organics in Marine Sediment, since both materials have 12 PCB congeners, five PAHs and five chlorinated pesticides in common. However, the concentrations differ by an order of magnitude for PAHs, and from one to over two orders of magnitude for the PCB congeners and chlorinated pesticides.     

Recent developments in food-matrix Reference Materials at NIST

Since 1996, the National Institute of Standards and Technology (NIST) has developed several food-matrix Standard Reference Materials (SRMs) characterized for nutrient concentrations. These include SRM 1544 Fatty Acids and Cholesterol in a Frozen Diet Composite, SRM 1546 Meat Homogenate, SRM 1548a Typical Diet, SRM 1566b Oyster Tissue, SRM 1846 Infant Formula, and SRM 2383 Baby Food Composite. Three additional materials--SRM 1946 Lake Superior Fish Tissue, SRM 2384 Baking Chocolate, and SRM 2385 Spinach--are in preparation. NIST also recently assigned values for proximate (fat, protein, etc.), individual fatty acid, and total dietary fiber concentrations in a number of existing SRMs and reference materials (RMs) that previously had values assigned for their elemental composition. NIST has used several modes for assignment of analyte concentrations in the food-matrix RMs, including the use of data provided by collaborating laboratories, alone and in combination with NIST data. The use of data provided by collaborating food industry and contract laboratories for the analysis of food-matrix RMs has enabled NIST to provide assigned values for many analytes that NIST does not have the resources or analytical expertise to measure.     

Standard reference materials for foods and dietary supplements

Well-characterized certified reference materials are needed by laboratories in the food testing, dietary supplement, and nutrition communities to facilitate compliance with labeling laws and improve the accuracy of information provided on product labels, so that consumers can make good choices. As a result of the enactment of the Nutrition Labeling and Education Act of 1990 and the Infant Formula Act of 1980, the National Institute of Standards and Technology (NIST) worked to develop a series of food-matrix standard reference materials (SRMs) characterized for nutrient concentrations. These include SRM 1544 Fatty Acids and Cholesterol in a Frozen Diet Composite, SRM 1546 Meat Homogenate, SRM 1548a Typical Diet, SRM 1566b Oyster Tissue, SRM 1846 Infant Formula, SRM 1946 Lake Superior Fish Tissue, SRM 1947 Lake Michigan Fish Tissue, SRM 2383 Baby Food Composite, SRM 2384 Baking Chocolate, SRM 2385 Slurried Spinach, and SRM 2387 Peanut Butter. With the enactment of the Dietary Supplement Health and Education Act of 1994, NIST has been working to develop suites of dietary supplement SRMs characterized for active and marker compounds and for toxic elements and pesticides, where appropriate. An updated SRM 1588b Organics in Cod Liver Oil, a suite of ephedra-containing materials (SRMs 3240–3245), a carrot extract in oil (SRM 3276), and a suite of ginkgo-containing materials (SRMs 3246–3248) are available. Several other materials are currently in preparation. Dietary supplements are sometimes provided in forms that are food-like; for these, values may also be assigned for nutrients, for example SRM 3244 Ephedra-Containing Protein Powder. Both the food-matrix and dietary supplement reference materials are intended primarily for validation of analytical methods. They may also be used as “primary control materials” in assignment of values to in-house (secondary) control materials to confirm accuracy and to establish measurement traceability to NIST.     

Quantitative analysis of selected PCB congeners in marine matrix reference materials using a novel cyanobiphenyl stationary phase

A novel p,p-cyanobiphenyl stationary phase (p-cyanobiphenyl, p-allyloxy methylpolysiloxane) has been evaluated for the GC investigation of polychlorinated biphenyls (PCBs). Several PCB congeners which coelute on the phases typically used for PCB analysis (e.g. 5% phenyl methylpolysiloxane) are separated on the p,p-cyanobiphenyl phase, including the hexachlorobiphenyl congeners PCB 163, PCB 164, and PCB 138. In this work, a p,p-cyanobiphenyl stationary phase was used to measure selected PCB congeners in two Standard Reference Materials (SRMs) available from the National Institute of Standards and Technology (NIST), and two Certified Reference Materials (CRMs) available from the Community Bureau of Reference (BCR). The materials analyzed were SRM 1588, Organics in Cod Liver Oil; SRM 1945, Organics in Whale Blubber; CRM 349, Chlorobiphenyls in Cod Liver Oil; and CRM 350, Chlorobiphenyls in Mackerel Oil. Concentrations are reported for several PCB congeners which coelute on the 5% phenyl methylpolysiloxane, including PCB 163 and PCB 164.