Toward Reliable Lipoprotein Particle Predictions from NMR Spectra of Human Blood

An Interlaboratory Ring Test

Sandra Monsonis Centelles*, Huub C.J. Hoefsloot, Bekzod Khakimov, Parvaneh Ebrahimi, Mads V. Lind, Mette Kristensen, Niels De Roo, Doris M. Jacobs, John Van Duynhoven, Claire Cannet, Fang Fang, Eberhard Humpfer, Hartmut Schäfer, Manfred Spraul, Søren B. Engelsen, Age K. Smilde

*Corresponding author for this work

Research output: Contribution to journalArticleAcademicpeer-review

9 Citations (Scopus)

Abstract

Lipoprotein profiling of human blood by 1H nuclear magnetic resonance (NMR) spectroscopy is a rapid and promising approach to monitor health and disease states in medicine and nutrition. However, lack of standardization of measurement protocols has prevented the use of NMR-based lipoprotein profiling in metastudies. In this study, a standardized NMR measurement protocol was applied in a ring test performed across three different laboratories in Europe on plasma and serum samples from 28 individuals. Data was evaluated in terms of (i) spectral differences, (ii) differences in LPD predictions obtained using an existing prediction model, and (iii) agreement of predictions with cholesterol concentrations in high- and low-density lipoproteins (HDL and LDL) particles measured by standardized clinical assays. ANOVA-simultaneous component analysis (ASCA) of the ring test spectral ensemble that contains methylene and methyl peaks (1.4-0.6 ppm) showed that 97.99% of the variance in the data is related to subject, 1.62% to sample type (serum or plasma), and 0.39% to laboratory. This interlaboratory variation is in fact smaller than the maximum acceptable intralaboratory variation on quality control samples. It is also shown that the reproducibility between laboratories is good enough for the LPD predictions to be exchangeable when the standardized NMR measurement protocol is followed. With the successful implementation of this protocol, which results in reproducible prediction of lipoprotein distributions across laboratories, a step is taken toward bringing NMR more into scope of prognostic and diagnostic biomarkers, reducing the need for less efficient methods such as ultracentrifugation or high-performance liquid chromatography (HPLC).
Original languageEnglish
Pages (from-to)8004-8012
JournalAnalytical Chemistry
Volume89
Issue number15
DOIs
Publication statusPublished - 2017

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Lipoproteins
Blood
Nuclear magnetic resonance
Magnetic resonance measurement
Plasmas
High performance liquid chromatography
Biomarkers
Nutrition
Analysis of variance (ANOVA)
LDL Lipoproteins
Standardization
Nuclear magnetic resonance spectroscopy
Medicine
Quality control
Assays
Cholesterol
Health

Cite this

Monsonis Centelles, S., Hoefsloot, H. C. J., Khakimov, B., Ebrahimi, P., Lind, M. V., Kristensen, M., ... Smilde, A. K. (2017). Toward Reliable Lipoprotein Particle Predictions from NMR Spectra of Human Blood: An Interlaboratory Ring Test. Analytical Chemistry, 89(15), 8004-8012. https://doi.org/10.1021/acs.analchem.7b01329
Monsonis Centelles, Sandra ; Hoefsloot, Huub C.J. ; Khakimov, Bekzod ; Ebrahimi, Parvaneh ; Lind, Mads V. ; Kristensen, Mette ; De Roo, Niels ; Jacobs, Doris M. ; Van Duynhoven, John ; Cannet, Claire ; Fang, Fang ; Humpfer, Eberhard ; Schäfer, Hartmut ; Spraul, Manfred ; Engelsen, Søren B. ; Smilde, Age K. / Toward Reliable Lipoprotein Particle Predictions from NMR Spectra of Human Blood : An Interlaboratory Ring Test. In: Analytical Chemistry. 2017 ; Vol. 89, No. 15. pp. 8004-8012.
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abstract = "Lipoprotein profiling of human blood by 1H nuclear magnetic resonance (NMR) spectroscopy is a rapid and promising approach to monitor health and disease states in medicine and nutrition. However, lack of standardization of measurement protocols has prevented the use of NMR-based lipoprotein profiling in metastudies. In this study, a standardized NMR measurement protocol was applied in a ring test performed across three different laboratories in Europe on plasma and serum samples from 28 individuals. Data was evaluated in terms of (i) spectral differences, (ii) differences in LPD predictions obtained using an existing prediction model, and (iii) agreement of predictions with cholesterol concentrations in high- and low-density lipoproteins (HDL and LDL) particles measured by standardized clinical assays. ANOVA-simultaneous component analysis (ASCA) of the ring test spectral ensemble that contains methylene and methyl peaks (1.4-0.6 ppm) showed that 97.99{\%} of the variance in the data is related to subject, 1.62{\%} to sample type (serum or plasma), and 0.39{\%} to laboratory. This interlaboratory variation is in fact smaller than the maximum acceptable intralaboratory variation on quality control samples. It is also shown that the reproducibility between laboratories is good enough for the LPD predictions to be exchangeable when the standardized NMR measurement protocol is followed. With the successful implementation of this protocol, which results in reproducible prediction of lipoprotein distributions across laboratories, a step is taken toward bringing NMR more into scope of prognostic and diagnostic biomarkers, reducing the need for less efficient methods such as ultracentrifugation or high-performance liquid chromatography (HPLC).",
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Monsonis Centelles, S, Hoefsloot, HCJ, Khakimov, B, Ebrahimi, P, Lind, MV, Kristensen, M, De Roo, N, Jacobs, DM, Van Duynhoven, J, Cannet, C, Fang, F, Humpfer, E, Schäfer, H, Spraul, M, Engelsen, SB & Smilde, AK 2017, 'Toward Reliable Lipoprotein Particle Predictions from NMR Spectra of Human Blood: An Interlaboratory Ring Test', Analytical Chemistry, vol. 89, no. 15, pp. 8004-8012. https://doi.org/10.1021/acs.analchem.7b01329

Toward Reliable Lipoprotein Particle Predictions from NMR Spectra of Human Blood : An Interlaboratory Ring Test. / Monsonis Centelles, Sandra; Hoefsloot, Huub C.J.; Khakimov, Bekzod; Ebrahimi, Parvaneh; Lind, Mads V.; Kristensen, Mette; De Roo, Niels; Jacobs, Doris M.; Van Duynhoven, John; Cannet, Claire; Fang, Fang; Humpfer, Eberhard; Schäfer, Hartmut; Spraul, Manfred; Engelsen, Søren B.; Smilde, Age K.

In: Analytical Chemistry, Vol. 89, No. 15, 2017, p. 8004-8012.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - Toward Reliable Lipoprotein Particle Predictions from NMR Spectra of Human Blood

T2 - An Interlaboratory Ring Test

AU - Monsonis Centelles, Sandra

AU - Hoefsloot, Huub C.J.

AU - Khakimov, Bekzod

AU - Ebrahimi, Parvaneh

AU - Lind, Mads V.

AU - Kristensen, Mette

AU - De Roo, Niels

AU - Jacobs, Doris M.

AU - Van Duynhoven, John

AU - Cannet, Claire

AU - Fang, Fang

AU - Humpfer, Eberhard

AU - Schäfer, Hartmut

AU - Spraul, Manfred

AU - Engelsen, Søren B.

AU - Smilde, Age K.

PY - 2017

Y1 - 2017

N2 - Lipoprotein profiling of human blood by 1H nuclear magnetic resonance (NMR) spectroscopy is a rapid and promising approach to monitor health and disease states in medicine and nutrition. However, lack of standardization of measurement protocols has prevented the use of NMR-based lipoprotein profiling in metastudies. In this study, a standardized NMR measurement protocol was applied in a ring test performed across three different laboratories in Europe on plasma and serum samples from 28 individuals. Data was evaluated in terms of (i) spectral differences, (ii) differences in LPD predictions obtained using an existing prediction model, and (iii) agreement of predictions with cholesterol concentrations in high- and low-density lipoproteins (HDL and LDL) particles measured by standardized clinical assays. ANOVA-simultaneous component analysis (ASCA) of the ring test spectral ensemble that contains methylene and methyl peaks (1.4-0.6 ppm) showed that 97.99% of the variance in the data is related to subject, 1.62% to sample type (serum or plasma), and 0.39% to laboratory. This interlaboratory variation is in fact smaller than the maximum acceptable intralaboratory variation on quality control samples. It is also shown that the reproducibility between laboratories is good enough for the LPD predictions to be exchangeable when the standardized NMR measurement protocol is followed. With the successful implementation of this protocol, which results in reproducible prediction of lipoprotein distributions across laboratories, a step is taken toward bringing NMR more into scope of prognostic and diagnostic biomarkers, reducing the need for less efficient methods such as ultracentrifugation or high-performance liquid chromatography (HPLC).

AB - Lipoprotein profiling of human blood by 1H nuclear magnetic resonance (NMR) spectroscopy is a rapid and promising approach to monitor health and disease states in medicine and nutrition. However, lack of standardization of measurement protocols has prevented the use of NMR-based lipoprotein profiling in metastudies. In this study, a standardized NMR measurement protocol was applied in a ring test performed across three different laboratories in Europe on plasma and serum samples from 28 individuals. Data was evaluated in terms of (i) spectral differences, (ii) differences in LPD predictions obtained using an existing prediction model, and (iii) agreement of predictions with cholesterol concentrations in high- and low-density lipoproteins (HDL and LDL) particles measured by standardized clinical assays. ANOVA-simultaneous component analysis (ASCA) of the ring test spectral ensemble that contains methylene and methyl peaks (1.4-0.6 ppm) showed that 97.99% of the variance in the data is related to subject, 1.62% to sample type (serum or plasma), and 0.39% to laboratory. This interlaboratory variation is in fact smaller than the maximum acceptable intralaboratory variation on quality control samples. It is also shown that the reproducibility between laboratories is good enough for the LPD predictions to be exchangeable when the standardized NMR measurement protocol is followed. With the successful implementation of this protocol, which results in reproducible prediction of lipoprotein distributions across laboratories, a step is taken toward bringing NMR more into scope of prognostic and diagnostic biomarkers, reducing the need for less efficient methods such as ultracentrifugation or high-performance liquid chromatography (HPLC).

U2 - 10.1021/acs.analchem.7b01329

DO - 10.1021/acs.analchem.7b01329

M3 - Article

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SP - 8004

EP - 8012

JO - Analytical Chemistry

JF - Analytical Chemistry

SN - 0003-2700

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Monsonis Centelles S, Hoefsloot HCJ, Khakimov B, Ebrahimi P, Lind MV, Kristensen M et al. Toward Reliable Lipoprotein Particle Predictions from NMR Spectra of Human Blood: An Interlaboratory Ring Test. Analytical Chemistry. 2017;89(15):8004-8012. https://doi.org/10.1021/acs.analchem.7b01329