TY - JOUR A1 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471430 DO - https://doi.org/10.1088/0026-1394/56/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, X.M. A1 - Li, H.M. A1 - Zhang, Q.H. A1 - Lu, X.H. A1 - Li, S.Q. A1 - Koch, Matthias A1 - Polzer, J. A1 - Hackenber, R. A1 - Moniruzzaman, M. A1 - Khan, M. A1 - Kakoulides, E. A1 - Pak-Wing, K. A1 - Richy, A1 - Chi-Shing, N. A1 - Lu, T. A1 - Gui, E.M. A1 - Cheow, P.S. A1 - Teo, T.L. A1 - Rego, E. A1 - Garrido, B. A1 - Carvalho, L. A1 - Leal, R. A1 - Violante, F. A1 - Baek, S.Y. A1 - Lee, S. A1 - Choi, K. A1 - Kim, B. A1 - Bucar-Miklavcic, M. A1 - Hopley, C. A1 - Nammoonnoy, J. A1 - Murray, J. A1 - Wilson, W. A1 - Toman, B. A1 - Itoh, N. A1 - Gokcen, T. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K146 low-polarity analyte in high fat food: benzo a pyrene in olive oil N2 - The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix. KW - Metrology KW - CCQM KW - Food KW - PAH PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1a/08017 VL - 57 IS - 1a SP - 08017 AN - OPUS4-52435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jäger, Christian A1 - Groom, N. S. A1 - Bowe, Elizabeth A. A1 - Horner, A. A1 - Davies, M. Elisabeth A1 - Murray, Rachel C. A1 - Duer, M. J. T1 - Investigation of the Nature of the Protein-Mineral Interface in Bone by Solid-State NMR N2 - Hydrogen-bearing species in the bone mineral environment were investigated using solid-state NMR spectroscopy of powdered bone, deproteinated bone, and B-type carbonated apatite. Using magic-angle spinning and cross-polarization techniques three types of structurally-bound water were observed in these materials. Two of these water types occupy vacancies within the apatitic mineral crystal in synthetic carbonated apatite and deproteinated bone and serve to stabilize these defect-containing crystals. The third water was observed at the mineral surface in unmodified bone but not in deproteinated bone, suggesting a role for this water in mediating mineral-organic matrix interactions. Direct evidence of monohydrogen phosphate in a 1H NMR spectrum of unmodified bone is presented for the first time. We obtained clear evidence for the presence of hydroxide ion in deproteinated bone by 1H MAS NMR. A 1H-31P heteronuclear correlation experiment provided unambiguous evidence for hydroxide ion in unmodified bone as well. Hydroxide ion in both unmodified and deproteinated bone mineral was found to participate in hydrogen bonding with neighboring water molecules and ions. In unmodified bone mineral hydroxide ion was found, through a 1H-31P heteronuclear correlation experiment, to be confined to a small portion of the mineral crystal, probably the internal portion. KW - NMR KW - Bone KW - Protein-mineral-interface PY - 2005 DO - https://doi.org/10.1529/biophysj.105.070243 SN - 0897-4756 SN - 1520-5002 VL - 17 IS - 12 SP - 3059 EP - 3061 PB - American Chemical Society CY - Washington, DC AN - OPUS4-11010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maltsev, Sergey A1 - Duer, M.J. A1 - Murray, R.C. A1 - Jäger, Christian T1 - A solid-state NMR comparison of the mineral structure in bone from diseases joints in the horse N2 - In this work, subchondral cortical bone material is investigated from the joints of five horses, three of which presented with no clinical signs or radiographic signs of osteoarthritis and two of which suffered osteoarthritis joint disease, as judged by clinical and radiographic assessment and histological findings. The horse is a good model for osteoarthritis in humans, so the aim of this study is to use nuclear magnetic resonance (NMR) for a detailed investigation of the bone structure in bone material affected by osteoarthritis. In particular, we report on the assessment of the mineral structure of these samples as viewed by solid-state NMR. KW - Bone KW - Osteoarthritis KW - NMR PY - 2007 DO - https://doi.org/10.1007/s10853-007-1916-z SN - 0022-2461 SN - 1573-4803 VL - 42 IS - 21 SP - 8804 EP - 8810 PB - Springer Science + Business Media B.V. CY - Norwell, Mass. AN - OPUS4-17580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wise, Erica R. A1 - Maltsev, Sergey A1 - Davies, M.E. A1 - Duer, M.J. A1 - Jäger, Christian A1 - Loveridge, N. A1 - Murray, Rachel C. A1 - Reid, D.G. T1 - The Organic - Mineral Interface in Bone Is Predominantly Polysaccharide KW - NMR KW - Bone KW - Mineral-organic interface PY - 2007 DO - https://doi.org/10.1021/cm702054c SN - 0897-4756 SN - 1520-5002 VL - 19 IS - 21 SP - 5055 EP - 5057 PB - American Chemical Society CY - Washington, DC AN - OPUS4-17583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -