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Spe column

Manufactured by Agilent Technologies

The SPE column is a specialized laboratory equipment used for solid-phase extraction. It is designed to capture, separate, and purify target analytes from complex sample matrices.

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4 protocols using spe column

1

Quantitative Analysis of Compounds via LC-MS/MS

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The selected extract samples were prepared as solutions with the concentration of 50 μg/mL using LC-MS pure methanol and pretreated with Agilent SPE column before LC-MS/MS analysis.
The LC-MS/MS analyses were run on a Waters Acquity UHPLC-DAD-Xevo G2-XS Q-Tof liquid chromatography-mass spectrometer. Waters ACQUITY UPLC BEH RP18 (2.1 × 50 mm, 1.7 μm) column was used for the analysis. The sample injection volume was 1.0 μL. The aqueous solution containing 0.1% formic acid was used as mobile phase A, and mobile phase B was acetonitrile. The gradient elution condition was as follows: 30% B (0–0.5 min), 30–80% B (0.5–4.0 min), 80% B (4.0–7.0 min), 80–30% B (7.0–7.2 min), 30% B (7.2–8.5 min) at a flow rate of 0.3 mL/min. The range of MS scan was set to m/z 50–2,000, electrospray ionization, and positive ion mode. The MS parameters were as follows: ion source temperature, 120°C; Capillary, 2 KV; Sampling Cone, 40 V; Source Offset, 80 V; Desolvation temperature, 450°C; Cone Gas, 50 L/h; Desolvation Gas, 700 L/h.
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2

Evaluating Solubilizers for CBD Aqueous Solutions

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Oil-based carrier PIB and surfactants including polysorbate 20 (Tween 20), polysorbate 80 (Tween 80), and SLS were evaluated as a solubilizer of CBD into aqueous solution. In a falcon tube (Sigma, Burlington, MA, USA), CBD (5 mg) and surfactant (at a final concentration of 10%; w/w) were mixed with phosphate buffer saline (PBS; 12 mL). Solutions were thoroughly mixed and placed still at room temperature for 24 h. CBD in each solution was extracted with an SPE column (100 mg; Agilent Technologies) eluted with methanol for further HPLC analysis. The stability of CBD in Tween 20 aqueous solution (10%; w/w) at different pH conditions was determined by the HPLC analysis. CBD solutions (200 μg/mL) at different pH conditions (pH = 4, 5, 6, and 7) were prepared and kept at room temperature for 30 days. The concentration of CBD in each solution at different timepoints (day 1, 7, 14, and 30) was measured by HPLC analysis with a linear regression based on area under the curve (online suppl. Fig. S1 and S3).
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3

Characterization and Purification of Organic Compounds

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Example 1

A. General Methods

All starting materials used herein were commercially available or earlier described in the literature. The 1H and 13C NMR spectra were recorded either on Bruker 300, Bruker DPX400 or Varian +400 spectrometers operating at 300, 400 and 400 MHz for 1H NMR respectively, using TMS or the residual solvent signal as an internal reference, in deuterated chloroform as solvent unless otherwise indicated. All reported chemical shifts are in ppm on the delta-scale, and the fine splitting of the signals as appearing in the recordings is generally indicated, for example as s: singlet, br s: broad singlet, d: doublet, t: triplet, q: quartet, m: multiplet. Unless otherwise indicated, in the tables below, 1H NMR data was obtained at 400 MHz, using CDCl3 as the solvent. A summary the 1H NMR and liquid chromatograph mass spectral (LCMS) characteristics of representative compounds is provided in Tables 1 and 2.

Purification of products was carried out using Chem Elut Extraction Columns (Varian, cat #1219-8002), Mega BE-SI (Bond Elut Silica) SPE Columns (Varian, cat #12256018; 12256026; 12256034) or by flash chromatography in silica-filled glass columns.

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4

NMR Spectroscopy and Purification Protocols

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Example 1

A. General Methods

All starting materials used herein were commercially available or earlier described in the literature. The 1H and 13C NMR spectra were recorded either on Bruker 300, Bruker DPX400 or Varian+400 spectrometers operating at 300, 400 and 400 MHz for 1H NMR respectively, using TMS or the residual solvent signal as an internal reference, in deuterated chloroform as solvent unless otherwise indicated. All reported chemical shifts are in ppm on the delta-scale, and the fine splitting of the signals as appearing in the recordings is generally indicated, for example as s: singlet, br s: broad singlet, d: doublet, t: triplet, q: quartet, m: multiplet. Unless otherwise indicated, in the tables below, 1H NMR data was obtained at 400 MHz, using CDCl3 as the solvent. A summary the 1H NMR and liquid chromatograph mass spectral (LCMS) characteristics of representative compounds is provided in Tables 1 and 2.

Purification of products was carried out using Chem Elut Extraction Columns (Varian, cat #1219-8002), Mega BE-SI (Bond Elut Silica) SPE Columns (Varian, cat #12256018; 12256026; 12256034) or by flash chromatography in silica-filled glass columns.

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