Preprint Article Version 1 This version is not peer-reviewed

Beta-Hydroxybutyric Acid as a Template for the X-ray Powder Diffraction Analysis of Gamma-Hydroxybutyric Acid

Version 1 : Received: 22 July 2024 / Approved: 23 July 2024 / Online: 24 July 2024 (07:20:12 CEST)

How to cite: Marabello, D.; Canepa, C.; Cioci, A.; Benzi, P. Beta-Hydroxybutyric Acid as a Template for the X-ray Powder Diffraction Analysis of Gamma-Hydroxybutyric Acid. Preprints 2024, 2024071850. https://doi.org/10.20944/preprints202407.1850.v1 Marabello, D.; Canepa, C.; Cioci, A.; Benzi, P. Beta-Hydroxybutyric Acid as a Template for the X-ray Powder Diffraction Analysis of Gamma-Hydroxybutyric Acid. Preprints 2024, 2024071850. https://doi.org/10.20944/preprints202407.1850.v1

Abstract

In this paper we report the possibility of using the X-ray powder diffraction (XRPD) technique to detect the gamma-hydroxybutyric acid (GHB) as its sodium salt in different beverages but because it is not possible to freely buy them, beta-hydroxybutyric acid (BHB) and its sodium salt (NaBHB) were used as a model to fine tune an X-ray diffraction method for the qualitative analysis of the sodium salt of GHB. The method requires a small quantity of beverage, and an easy sample preparation, that consists only in the NaOH addition to the drink and a subsequent drying step. The dry residue obtained can be easily analyzed with XRPD using a single crystal X-ray diffractometer to exploit its high sensitivity that allows very fast patterns collection. Several beverages with different NaBHB:NaOH molar ratios were tested and the results show that NaBHB is detected in all drinks analyzed when NaBHB:NaOH molar ratio is 1:50 using characteristic peak at very low 2θ values that permits to detect its presence also in complex beverage matrices. Moreover, depending on the NaOH amount added, shifting and/or splitting of the characteristic peak of the NaBHB salt was observed, and the origin of this behavior was investigated.

Keywords

X-ray powder diffraction; non-destructive analysis; spiked beverages; γ-hydroxybutyric acid (GHB); β-hydroxybutyric acid (BHB); drink analysis

Subject

Chemistry and Materials Science, Other

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