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Determination of PAHs in Solution with a Single Reference Standard by a Combination of 1H Quantitative NMR Spectroscopy and Chromatography.
Anal Chem. 2017 07 05; 89(13):6963-6968.AC

Abstract

We have applied a combination of 1H quantitative NMR spectroscopy (1H-qNMR) and chromatography (GC or LC) to establish reliable analytical methods (qNMR/GC and qNMR/LC) for organic compounds. In this method, a reference standard is used as an internal standard for both 1H-qNMR and chromatography to estimate relative molar sensitivity (RMS) for analytes. The RMS values are calculated from the molar ratios between analytes and the reference standard obtained by 1H-qNMR; and the response ratio between them obtained by chromatography. Concentrations of analytes in the organic solution can be simultaneously determined from the RMS and amount of the reference standard added in the sample solution. This analytical method is an innovative one because only one reference standard with International System of Units (SI)-traceable property value, purity, or concentration, is necessary to determine accurate concentrations of multiple organic components in organic solutions, without the respective certified reference standards for various analytes. To verify this method, a certified reference material, NIST SRM 1647f, was used. Among the 16 polycyclic aromatic hydrocarbons (PAHs) included in NIST SRM 1647f, naphthalene and benzo[a]pyrene were selected as analytes for this method, using 1,4-bis(trimethylsilyl)benzene-d4 as the reference standard. Each quantitative value obtained by qNMR/GC and qNMR/LC agreed with each certified value within its expanded uncertainty.

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Authors+Show Affiliations

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology , 1-1-1, Umezono, Tsukuba, Ibaraki 305-8563, JAPAN.

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology , 1-1-1, Umezono, Tsukuba, Ibaraki 305-8563, JAPAN.

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology , 1-1-1, Umezono, Tsukuba, Ibaraki 305-8563, JAPAN.

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology , 1-1-1, Umezono, Tsukuba, Ibaraki 305-8563, JAPAN.

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology , 1-1-1, Umezono, Tsukuba, Ibaraki 305-8563, JAPAN.

National Institute of Health Sciences , 1-18-1, Kamiyoga, Setagaya-ku, Tokyo 158-8501, JAPAN.

National Institute of Health Sciences , 1-18-1, Kamiyoga, Setagaya-ku, Tokyo 158-8501, JAPAN.

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology , 1-1-1, Umezono, Tsukuba, Ibaraki 305-8563, JAPAN.

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology , 1-1-1, Umezono, Tsukuba, Ibaraki 305-8563, JAPAN.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

28581717

Citation

Kitamaki, Yuko, et al. "Determination of PAHs in Solution With a Single Reference Standard By a Combination of 1H Quantitative NMR Spectroscopy and Chromatography." Analytical Chemistry, vol. 89, no. 13, 2017, pp. 6963-6968.

Kitamaki Y, Saito N, Yamazaki T, et al. Determination of PAHs in Solution with a Single Reference Standard by a Combination of 1H Quantitative NMR Spectroscopy and Chromatography. Anal Chem. 2017;89(13):6963-6968.

Kitamaki, Y., Saito, N., Yamazaki, T., Otsuka, S., Nakamura, S., Nishizaki, Y., Sugimoto, N., Numata, M., & Ihara, T. (2017). Determination of PAHs in Solution with a Single Reference Standard by a Combination of 1H Quantitative NMR Spectroscopy and Chromatography. Analytical Chemistry, 89(13), 6963-6968. https://doi.org/10.1021/acs.analchem.6b05074

Kitamaki Y, et al. Determination of PAHs in Solution With a Single Reference Standard By a Combination of 1H Quantitative NMR Spectroscopy and Chromatography. Anal Chem. 2017 07 5;89(13):6963-6968. PubMed PMID: 28581717.

* Article titles in AMA citation format should be in sentence-case

TY - JOUR T1 - Determination of PAHs in Solution with a Single Reference Standard by a Combination of 1H Quantitative NMR Spectroscopy and Chromatography. AU - Kitamaki,Yuko, AU - Saito,Naoki, AU - Yamazaki,Taichi, AU - Otsuka,Satoko, AU - Nakamura,Satoe, AU - Nishizaki,Yuzo, AU - Sugimoto,Naoki, AU - Numata,Masahiko, AU - Ihara,Toshihide, Y1 - 2017/06/20/ PY - 2017/6/6/pubmed PY - 2017/6/6/medline PY - 2017/6/6/entrez SP - 6963 EP - 6968 JF - Analytical chemistry JO - Anal Chem VL - 89 IS - 13 N2 - We have applied a combination of 1H quantitative NMR spectroscopy (1H-qNMR) and chromatography (GC or LC) to establish reliable analytical methods (qNMR/GC and qNMR/LC) for organic compounds. In this method, a reference standard is used as an internal standard for both 1H-qNMR and chromatography to estimate relative molar sensitivity (RMS) for analytes. The RMS values are calculated from the molar ratios between analytes and the reference standard obtained by 1H-qNMR; and the response ratio between them obtained by chromatography. Concentrations of analytes in the organic solution can be simultaneously determined from the RMS and amount of the reference standard added in the sample solution. This analytical method is an innovative one because only one reference standard with International System of Units (SI)-traceable property value, purity, or concentration, is necessary to determine accurate concentrations of multiple organic components in organic solutions, without the respective certified reference standards for various analytes. To verify this method, a certified reference material, NIST SRM 1647f, was used. Among the 16 polycyclic aromatic hydrocarbons (PAHs) included in NIST SRM 1647f, naphthalene and benzo[a]pyrene were selected as analytes for this method, using 1,4-bis(trimethylsilyl)benzene-d4 as the reference standard. Each quantitative value obtained by qNMR/GC and qNMR/LC agreed with each certified value within its expanded uncertainty. SN - 1520-6882 UR - https://www.unboundmedicine.com/medline/citation/28581717/Determination_of_PAHs_in_Solution_with_a_Single_Reference_Standard_by_a_Combination_of_1H_Quantitative_NMR_Spectroscopy_and_Chromatography_ L2 - https://doi.org/10.1021/acs.analchem.6b05074 DB - PRIME DP - Unbound Medicine ER -