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3 protocols using deuterium oxide

1

NMR Analysis of Cystine and Sulfite

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All NMR experiments were carried out on a Bruker Avance III 600 MHz, Bruker Biospin GmbH, (Rheinstetten, Germany) with TXI probe and a temperature control unit was used for all 1D and 2D experiments. The 5-mm single use NMR tubes were purchased from GPE Scientific, Leighton Buzzard, UK) (product code 512-7). The spectra were recorded using Deuterium oxide (99.90% D) purchased from Fluorochem (Glossop, UK). l-cystine (≥ 99.7% by TLC) and sodium sulfite (≥98%) were purchased from Sigma-Aldrich, Haverhill, UK and used without further purification. Distilled H2O was generating using an ELGA water still and degassed using N2 gas (BOC, 99.99%)
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2

Synthesis of Rare-Earth Doped Nanoparticles

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1-Octadecene (ODE, technical grade, 90%),
triethyloxonium tetrafluoroborate ([Et3O][BF4], ≥97.0%), acetonitrile (ACN, 99.8%, anhydrous), chloroform
(≥99%, anhydrous), and methanol (≥99.9%, anhydrous)
were purchased from Sigma-Aldrich. Oleic acid (extra pure), trifluoroacetic
acid (HTFA, ≥99.0%, for HPLC), trifluoroacetic anhydride (TFAA,
≥99.0%), lithium carbonate (Li2CO3, 99.999%,
trace metal basis), yttrium oxide (Y2O3, 99.9999%,
REO), and ytterbium oxide (Yb2O3, 99.998%, REO)
were purchased from Fisher Scientific. Toluene (≥99.8%, anhydrous)
and ethanol (≥99.8%, anhydrous) were purchased from VWR Chemicals.
Hexane (>96.0%, anhydrous) was purchased from TCI. Deuterium oxide
(D2O, >99.90% D) was purchased from Fluorochem Ltd.
All chemicals were used as received unless specified differently.
All manipulations were performed under a N2 atmosphere
using standard Schlenk line techniques or a nitrogen-filled glove
box (<0.1 ppm H2O; <0.1 ppm O2) unless
otherwise mentioned.
Milli-Q water was obtained from a Milli-Q
Advantage A10 system
(Merck Millipore, 18.2 MΩ·cm, 2 ppb TOC).
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3

Analyzing Seized Novel Psychoactive Substances

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Methanol, acetonitrile, water, formic acid (FA) and trifluoroacetic acid (TFA), HPLC grade, dimethyl sulfoxide-d6 and isotopic purity 99.9 atom %D were purchased from Sigma-Aldrich (Dorset, UK). Methanol (LC-MS grade), t-butyl-methyl-ether (TBME), tripelennamine, quinolone were from Sigma-Aldrich (Dorset, UK). Deuterium oxide, isotopic purity 99.8 atom %D, was purchased from Fluorochem LTD (Derbyshire, UK). Three unknown street samples were received from TICTAC Communications Ltd (London, UK). The samples were test purchased as NPS from an overseas, open access website. Samples were kept in a locked cabinet at room temperature.
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