UHPLC-UV analysis was performed on a Shimadzu (Kyoto, Japan) Nexera system equipped with a DAD and employed a Phenomenex 1.7 µm XB-C18 column (50 mm × 2.1 mm). A Shimadzu LabSolutions software package was used for data analysis. Cannabinoids were separated with a H2O (0.1% formic acid) and ACN (0.1% formic acid) gradient. Starting with 5% ACN, the gradient was increased to 100 % ACN over 18 minutes. Preferred detection wavelengths were 210 and 273 nm. Semipreparative HPLC was performed on a Shimadzu HPLC (Kyoto, Japan) connected to a DAD detector (Shimadzu, model SPD-20A) and equipped with a YMC-Pack ODS-AQ (250 × 10 mm, S-5, 12 nm). The mobile phase was 70% and 80% ACN for polar and nonpolar fractions respectively. The flow rate was 3.0 mL/min.
Spd 20a
Manufactured by YMC
Sourced in Japan
The SPD-20A is a laboratory centrifuge designed for general-purpose applications. It is capable of high-speed separation of samples with a maximum speed of 20,000 rpm and a maximum relative centrifugal force (RCF) of 48,400 x g. The SPD-20A features a compact design and a user-friendly control panel for easy operation.
Automatically generated - may contain errors
Lab products found in correlation
Ods aq, by YMC (1 mentions)
1.7 m xb c18 column, by Phenomenex (1 mentions)
High performance liquid chromatography (hplc), by Shimadzu (1 mentions)
Avance 400 nmr spectrometer, by Bruker (1 mentions)
Du640 uv spectrophotometer, by Beckman Coulter (1 mentions)
Maxis uhr tof mass spectrometer, by Bruker (1 mentions)
Ods a column, by YMC (1 mentions)
P 1020 polarimeter, by Jasco (1 mentions)
J 715 spectropolarimeter, by Jasco (1 mentions)
Spectrum two ft ir spectrometer, by PerkinElmer (1 mentions)
Exactive spectrometer, by Thermo Fisher Scientific (1 mentions)
Lc 6ad, by Shimadzu (1 mentions)
Sephadex lh 20 gel, by GE Healthcare (1 mentions)
Silica gel, by Qingdao Marine Chemical (1 mentions)
Pack ods a column, by YMC (1 mentions)
Gf254 plates, by Qingdao Marine Chemical (1 mentions)
Atractylenolide 3, by Merck Group (1 mentions)
Atractylenolide 1, by Merck Group (1 mentions)
Lc 20ad, by YMC (1 mentions)
Triart c18 column, by YMC (1 mentions)
4 protocols using spd 20a
1
Cannabinoid Analysis by UHPLC-UV
2
Analytical Characterization of Organic Compounds
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Optical rotation values were recorded on a JASCO P-1020 polarimeter. CD spectra were recorded on a J-715 spectropolarimeter (JASCO, Gross-Umstadt, Germany). UV spectra were obtained on a Beckman DU-640 UV spectrophotometer. NMR spectra were recorded on a Bruker Avance 400 NMR spectrometer in CDCl3. High-resolution ESI mass spectra were performed on a Bruker maXis UHR-TOF mass spectrometer in positive ion mode. For column chromatography, silica gel (200–300 mesh, Qingdao Mar. Chem. Ind. Co. Ltd.) and RP C18 gel (YMC) were used. High-performance liquid chromatography (HPLC) was performed on a Shimadzu LC-6AD controller with an SPD-20A UV–vis detector equipped with YMC-Pack ODS-A columns (250 × 10 mm i.d., 5 μm and 250 × 4.6 mm i.d., 5 μm).
3
Characterization of Organic Compounds
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The NMR spectra were
recorded in CD3OD on a Bruker 400 MHz instrument (Bruker,
Karlsruhe, Germany), with tetramethylsilane as the internal standard.
HRESIMS data were obtained from a Thermo-Scientific Exactive spectrometer.
IR spectra (KBr) were recorded on a PerkinElmer Spectrum Two FT-IR
spectrometer. Silica gel (200–300 mesh; Qingdao Marine Chemical
Factory, China), MCI gel (CHP20, 75–150 μm; Mitsubishi
Chemical Corporation, Japan), ODS (50 μm; YMC, Japan), and Sephadex
LH-20 gel (Pharmacia Biotech, Sweden) were used for column chromatography.
Thin-layer chromatography was carried out on GF254 plates (Qingdao
Marine Chemical Factory). Preparative high-performance liquid chromatography
(HPLC) was carried out using a Shimadzu LC-6AD (Shimadzu, Japan) instrument
with a YMC-Pack ODS-A column (20 mm I.D. × 250 mm, S-5 μm,
12 nm) and an SPD-20A wavelength detector at 210 nm. HPLC solvents
were obtained from Tedia Company, Inc.
recorded in CD3OD on a Bruker 400 MHz instrument (Bruker,
Karlsruhe, Germany), with tetramethylsilane as the internal standard.
HRESIMS data were obtained from a Thermo-Scientific Exactive spectrometer.
IR spectra (KBr) were recorded on a PerkinElmer Spectrum Two FT-IR
spectrometer. Silica gel (200–300 mesh; Qingdao Marine Chemical
Factory, China), MCI gel (CHP20, 75–150 μm; Mitsubishi
Chemical Corporation, Japan), ODS (50 μm; YMC, Japan), and Sephadex
LH-20 gel (Pharmacia Biotech, Sweden) were used for column chromatography.
Thin-layer chromatography was carried out on GF254 plates (Qingdao
Marine Chemical Factory). Preparative high-performance liquid chromatography
(HPLC) was carried out using a Shimadzu LC-6AD (Shimadzu, Japan) instrument
with a YMC-Pack ODS-A column (20 mm I.D. × 250 mm, S-5 μm,
12 nm) and an SPD-20A wavelength detector at 210 nm. HPLC solvents
were obtained from Tedia Company, Inc.
4
Atractylenolide Analysis by HPLC
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Samples were analyzed by a reverse-phase HPLC system (Shimadzu 20A, Kyoto, Japan) that consisted of an autosampler (SIL-20A), a binary pump (LC-20AD), and a photodiode array detector (SPD-20A) and was equipped with a YMC-Triart C18 column (5 μm × 4.6 mm × 250 mm) (YMC, Kyoto, Japan). Gradient flows for the two-solvent system (solvent A, 0.05% phosphoric acid in water; solvent B, acetonitrile) were as follows: 85% A/15% B at 0 min, 85% A/15% B at 5 min, 50% A/50% B at 15 min, 50% A/50% B at 20 min, 40% A/60% B at 25 min, 40% A/60% B at 30 min, 15% A/85% at 35 min, 15% A/85% at 40 min, 85% A/15% at 42 min, and 85% A/15% at 45 min. The flow rate of the mobile phase was 1.0 ml/min with an injection volume of 10 μl. Detection was performed at 220 nm for atractylenolide III (Sigma, St. Louis, MO, USA) or at 280 nm for atractylenolide I (Sigma).
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