Quantification of endocannabinoids in human cerebrospinal fluid using a novel micro-flow liquid chromatography-mass spectrometry method

Bingshu He; Xinyu Di; Faisa Guled; Aster V.E. Harder; Arn M.J.M. van den Maagdenberg; Gisela M. Terwindt; Elke H.J. Krekels; Isabelle Kohler; Amy Harms; Rawi Ramautar; Thomas Hankemeier

doi:10.1016/j.aca.2022.339888

Quantification of endocannabinoids in human cerebrospinal fluid using a novel micro-flow liquid chromatography-mass spectrometry method

Bingshu He, Xinyu Di, Faisa Guled, Aster V.E. Harder, Arn M.J.M. van den Maagdenberg, Gisela M. Terwindt, Elke H.J. Krekels, Isabelle Kohler, Amy Harms, Rawi Ramautar^*, Thomas Hankemeier

^*Corresponding author for this work

Research output: Contribution to Journal › Article › Academic › peer-review

Abstract

The endocannabinoid system (ECS) is implicated in various brain disorders. Changes in the composition of the cerebrospinal fluid (CSF) may be associated with ECS-related pathologies. Endocannabinoids (eCBs) and their analogues are present at low concentrations in human CSF, which hampered the investigation of the ECS in this body fluid. In this study, we developed a highly sensitive and selective micro-flow liquid chromatography-tandem mass spectrometry (micro-LC-MS/MS) method for the analysis of eCBs and eCB analogues in human CSF. The developed method allowed for the quantitative analysis of 16 eCBs and their analogues in human CSF. Micro-LC-MS/MS analyses were performed at a flow-rate of 4 μL min⁻¹ with a 0.3-mm inner diameter column. A minor modification of a novel spray needle was carried out to improve the robustness of our method. By using an injection volume of 3 μL, our method reached limits of detection in the range from 0.6 to 1293.4 pM and limits of quantification in range from 2.0 to 4311.3 pM while intra- and interday precisions were below 13.7%. The developed workflow was successfully used for the determination of eCBs in 288 human CSF samples. It is anticipated that the proposed approach will contribute to a deeper understanding of the role of ECS in various brain disorders.

Original language	English
Article number	339888
Pages (from-to)	1-9
Number of pages	9
Journal	Analytica Chimica Acta
Volume	1210
Early online date	2 May 2022
DOIs	https://doi.org/10.1016/j.aca.2022.339888
Publication status	Published - 1 Jun 2022

Bibliographical note

Funding Information:
This study was supported by the China Scholarship Council ( CSC , No. 201906390032 to Bingshu He and CSC , No. 201707060012 to Xinyu Di). Dr. Rawi Ramautar would like to acknowledge the financial support of the Vidi grant scheme of the Netherlands Organization of Scientific Research ( NWO Vidi 723.016.003 ). This work was also supported by the Netherlands Organization for Health Research and Development (Vidi grant no. 917-11-31 to GMT), and European Community (EC) funded FP7-EUROHEADPAIN (grant no. 602633 to AMJMvdM). This research was part of the Netherlands X-omics Initiative and partially funded by NWO , project 184.034.019 .

Publisher Copyright:
© 2022 The Authors

Keywords

Cerebrospinal fluid
Down-scaling analysis
Endocannabinoids
Micro-LC-MS

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10.1016/j.aca.2022.339888

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He, B., Di, X., Guled, F., Harder, A. V. E., van den Maagdenberg, A. M. J. M., Terwindt, G. M., Krekels, E. H. J., Kohler, I., Harms, A., Ramautar, R., & Hankemeier, T. (2022). Quantification of endocannabinoids in human cerebrospinal fluid using a novel micro-flow liquid chromatography-mass spectrometry method. Analytica Chimica Acta, 1210, 1-9. Article 339888. https://doi.org/10.1016/j.aca.2022.339888

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abstract = "The endocannabinoid system (ECS) is implicated in various brain disorders. Changes in the composition of the cerebrospinal fluid (CSF) may be associated with ECS-related pathologies. Endocannabinoids (eCBs) and their analogues are present at low concentrations in human CSF, which hampered the investigation of the ECS in this body fluid. In this study, we developed a highly sensitive and selective micro-flow liquid chromatography-tandem mass spectrometry (micro-LC-MS/MS) method for the analysis of eCBs and eCB analogues in human CSF. The developed method allowed for the quantitative analysis of 16 eCBs and their analogues in human CSF. Micro-LC-MS/MS analyses were performed at a flow-rate of 4 μL min−1 with a 0.3-mm inner diameter column. A minor modification of a novel spray needle was carried out to improve the robustness of our method. By using an injection volume of 3 μL, our method reached limits of detection in the range from 0.6 to 1293.4 pM and limits of quantification in range from 2.0 to 4311.3 pM while intra- and interday precisions were below 13.7%. The developed workflow was successfully used for the determination of eCBs in 288 human CSF samples. It is anticipated that the proposed approach will contribute to a deeper understanding of the role of ECS in various brain disorders.",

keywords = "Cerebrospinal fluid, Down-scaling analysis, Endocannabinoids, Micro-LC-MS",

author = "Bingshu He and Xinyu Di and Faisa Guled and Harder, {Aster V.E.} and {van den Maagdenberg}, {Arn M.J.M.} and Terwindt, {Gisela M.} and Krekels, {Elke H.J.} and Isabelle Kohler and Amy Harms and Rawi Ramautar and Thomas Hankemeier",

note = "Funding Information: This study was supported by the China Scholarship Council ( CSC , No. 201906390032 to Bingshu He and CSC , No. 201707060012 to Xinyu Di). Dr. Rawi Ramautar would like to acknowledge the financial support of the Vidi grant scheme of the Netherlands Organization of Scientific Research ( NWO Vidi 723.016.003 ). This work was also supported by the Netherlands Organization for Health Research and Development (Vidi grant no. 917-11-31 to GMT), and European Community (EC) funded FP7-EUROHEADPAIN (grant no. 602633 to AMJMvdM). This research was part of the Netherlands X-omics Initiative and partially funded by NWO , project 184.034.019 . Publisher Copyright: {\textcopyright} 2022 The Authors",

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He, B, Di, X, Guled, F, Harder, AVE, van den Maagdenberg, AMJM, Terwindt, GM, Krekels, EHJ, Kohler, I, Harms, A, Ramautar, R & Hankemeier, T 2022, 'Quantification of endocannabinoids in human cerebrospinal fluid using a novel micro-flow liquid chromatography-mass spectrometry method', Analytica Chimica Acta, vol. 1210, 339888, pp. 1-9. https://doi.org/10.1016/j.aca.2022.339888

TY - JOUR

T1 - Quantification of endocannabinoids in human cerebrospinal fluid using a novel micro-flow liquid chromatography-mass spectrometry method

AU - He, Bingshu

AU - Di, Xinyu

AU - Guled, Faisa

AU - Harder, Aster V.E.

AU - van den Maagdenberg, Arn M.J.M.

AU - Terwindt, Gisela M.

AU - Krekels, Elke H.J.

AU - Kohler, Isabelle

AU - Harms, Amy

AU - Ramautar, Rawi

AU - Hankemeier, Thomas

N1 - Funding Information: This study was supported by the China Scholarship Council ( CSC , No. 201906390032 to Bingshu He and CSC , No. 201707060012 to Xinyu Di). Dr. Rawi Ramautar would like to acknowledge the financial support of the Vidi grant scheme of the Netherlands Organization of Scientific Research ( NWO Vidi 723.016.003 ). This work was also supported by the Netherlands Organization for Health Research and Development (Vidi grant no. 917-11-31 to GMT), and European Community (EC) funded FP7-EUROHEADPAIN (grant no. 602633 to AMJMvdM). This research was part of the Netherlands X-omics Initiative and partially funded by NWO , project 184.034.019 . Publisher Copyright: © 2022 The Authors

PY - 2022/6/1

Y1 - 2022/6/1

N2 - The endocannabinoid system (ECS) is implicated in various brain disorders. Changes in the composition of the cerebrospinal fluid (CSF) may be associated with ECS-related pathologies. Endocannabinoids (eCBs) and their analogues are present at low concentrations in human CSF, which hampered the investigation of the ECS in this body fluid. In this study, we developed a highly sensitive and selective micro-flow liquid chromatography-tandem mass spectrometry (micro-LC-MS/MS) method for the analysis of eCBs and eCB analogues in human CSF. The developed method allowed for the quantitative analysis of 16 eCBs and their analogues in human CSF. Micro-LC-MS/MS analyses were performed at a flow-rate of 4 μL min−1 with a 0.3-mm inner diameter column. A minor modification of a novel spray needle was carried out to improve the robustness of our method. By using an injection volume of 3 μL, our method reached limits of detection in the range from 0.6 to 1293.4 pM and limits of quantification in range from 2.0 to 4311.3 pM while intra- and interday precisions were below 13.7%. The developed workflow was successfully used for the determination of eCBs in 288 human CSF samples. It is anticipated that the proposed approach will contribute to a deeper understanding of the role of ECS in various brain disorders.

AB - The endocannabinoid system (ECS) is implicated in various brain disorders. Changes in the composition of the cerebrospinal fluid (CSF) may be associated with ECS-related pathologies. Endocannabinoids (eCBs) and their analogues are present at low concentrations in human CSF, which hampered the investigation of the ECS in this body fluid. In this study, we developed a highly sensitive and selective micro-flow liquid chromatography-tandem mass spectrometry (micro-LC-MS/MS) method for the analysis of eCBs and eCB analogues in human CSF. The developed method allowed for the quantitative analysis of 16 eCBs and their analogues in human CSF. Micro-LC-MS/MS analyses were performed at a flow-rate of 4 μL min−1 with a 0.3-mm inner diameter column. A minor modification of a novel spray needle was carried out to improve the robustness of our method. By using an injection volume of 3 μL, our method reached limits of detection in the range from 0.6 to 1293.4 pM and limits of quantification in range from 2.0 to 4311.3 pM while intra- and interday precisions were below 13.7%. The developed workflow was successfully used for the determination of eCBs in 288 human CSF samples. It is anticipated that the proposed approach will contribute to a deeper understanding of the role of ECS in various brain disorders.

KW - Cerebrospinal fluid

KW - Down-scaling analysis

KW - Endocannabinoids

KW - Micro-LC-MS

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JO - Analytica Chimica Acta

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Quantification of endocannabinoids in human cerebrospinal fluid using a novel micro-flow liquid chromatography-mass spectrometry method

Abstract

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Keywords

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