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Lux cellulose 4

Manufactured by Phenomenex
Sourced in United States

The Lux Cellulose-4 is a high-performance liquid chromatography (HPLC) column designed for the separation and analysis of a wide range of chiral compounds. It features a cellulose-based stationary phase that provides efficient and selective separation of enantiomers.

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6 protocols using lux cellulose 4

1

Separation of Silybin Derivatives

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The separation of 2,3-dehydrosilybin A and 2,3-dehydrosilybin B was achieved on Lux 3μ Cellulose-4 (2 × 50 mm, particle size 3 µm) column (Phenomenex, Torrance, CA, USA) equipped with security guard cartridge Lux Cellulose-4 (4 × 2.0 mm, 3 μm, Phenomenex, Torrance, CA, USA). Binary gradient elution: Mobile phase A: 10% acetonitrile, 0.1% formic acid; mobile phase B: 80% acetonitrile, 0.1% formic acid; gradient: 0 min 30% B, 0–12 min 30–50% B, 12–13 min 50–30% B, 13–15 min 30% B to equilibrate the column; flow rate 0.5 mL/min, t = 25 °C. The sample was dissolved in methanol and injection volume was 1 μL.
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2

Chiral HPLC Analysis of Compounds 2 and 5

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Chiral HPLC analysis of compound 2 was conducted by using a chiral column (Lux Cellulose-3, 5 μm, 250 × 4.6 mm, phenomenex) with UV detection at 265 nm under the following program: solvent system (solvent A, 10% CH3CN in water; solvent B, 90% CH3CN in water); 38% B (0–35 min), flow rate at 1 mL min−1. Chiral HPLC analysis of compound 5 was conducted by using a chiral column (Lux Cellulose-4, 5 μm, 250 × 4.6 mm, phenomenex) with UV detection at 265 nm under the following program: solvent system (solvent A, 10% CH3CN in water; solvent B, 90% CH3CN in water); 5% B to 100% B (0–20 min), 100% B (21−25 min), 100% B to 5%B (25−26 min), 5% B (26–30 min), flow rate at 1 mL min−1.
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3

Chiral Analysis of Naringenin by UPLC-MS/MS

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UPLC-MS/MS analysis was performed on Sciex 5500+ triple quadrupole mass spectrometer equipped with an ESI source and an Exionlc ad system ultra-high performance liquid chromatography (AB SCIEX, USA). The system was controlled and the data were collected using the SCIEX Analyst OS software package (version 1.7.1). The data were analyzed using the SCIEX OS software package (version 2.0.0.45330).
Chromatographic separation of naringenin was performed on six chiral analytical columns. Cellulose tris (3,5-dimethylphenylcarbamate) (Lux Cellulose-1), cellulose tris (3-chloro-4-methylphenylcarbamate) (Lux Cellulose-2), cellulose tris (4-methylbenzoate) (Lux Cellulose-3), and cellulose tris (4-chloro-3-methylphenylcarbamate) (Lux Cellulose-4) were purchased from Phenomenex (Torrance, USA). Amylose-tris (3-chloro-5-methylphenyl carbamate) (Chiralpak IG-3) was purchased from Daicel (Tokyo, Japan). All five columns were sized 150 mm × 2.0 mm i.d. packed with 3-μm particles. Hydroxypropyl-β-cyclodextrin (InfinityLab Poroshell 120 Chiral-CD) was purchased from Agilent (CA, USA), and the column was sized 150 mm × 2.1 mm i. d. packed with 2.7-μm particles.
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4

Chiral SFC Separation Protocol

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Chiral-phase SFC screening and optimization experiments were carried out on Waters Acquity UPC2 systems equipped with a fluid delivery module (a liquid CO2 pump and a modifier pump), a sampler manager–FL autosampler, two auxiliary column managers allowing six installed columns, a photodiode array detector, and MassLynx software. Columns packed with Chiralpak (AD-3, AS-3, IA, IB, IC, IE, IF) and Chiralcel (OD-3, OJ-3, OZ-3) were purchased from Chiral Technologies; Lux Amylose-2 and Lux Cellulose-4 columns were purchased from Phenomenex. Dimensions and particle size for all columns were 4.6 × 150 mm, 3 μm. Chiral SFC separations were carried out on the diverse set of columns described above by gradient elution at a flow rate of 3 mL/min with the back-pressure regulator set at 200 bar. The SFC eluents were solvent A (CO2) and solvent B (25 mM isobutylamine in MeOH). The mobile phases were programmed as follows: linear gradient from 1% to 40% B in 5 min; hold at 40% B for 1 min. The column and samples were maintained at a temperature of 40 and 20 °C, respectively.
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5

Chiral Compound Separation and Analysis

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Example 124

The R and S enantiomers of racemic compounds and the diastereomers (including cis- and trans-) of compounds were separated using either Chiral SFC or Chiral HPLC or preparative HPLC or SFC utilizing different columns such as XBridge Shield RP18 OBD, (CHIRALCEL OJ, CHIRALCEL OD, ChiralPAK AD, (R,R)-WHELK-O1-Kromasil, ChiralPAK IA, ChiralPAK IC, ChiralPAK ID, Lux Cellulose-4, SHIMADZU-SPD-20A, Phenomenex Lux, Cellulose-4, Amchemteq ACl Am-1 with different dimensions and diameter.

Columns were eluted with two mobile phases (Phase A and Phase B) with gradient from 0 to 100% for both phases. Some examples of phases used but not limited: 0.1% diethylamine in MeOH, water (0.05% TFA), MeCN, Hexane (0.1% diethylamine or diisopropylamine), MeOH, dichloromethane, isopropanol, ethanol, MTBE, 0.2% isopropanol in EtOH, 0.1% isopropanol in hexane, 0.1% aqueous diethyl amine, 0.1% or 0.2% 2,6-diethylaniline in tert butyl methyl ether. Peaks were detected at 220 and 254 nm.

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6

Chiral Separation Techniques for Racemic Compounds

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Example 124

The R and S enantiomers of racemic compounds and the diastereomers (including cis- and trans-) of compounds were separated using either Chiral SFC or Chiral HPLC or preparative HPLC or SFC utilizing different columns such as XBridge Shield RP18 OBD, (CHIRALCEL OJ, CHIRALCEL OD, ChiralPAK AD, (R,R)-WHELK-O1-Kromasil, ChiralPAK IA, ChiralPAK IC, ChiralPAK ID, Lux Cellulose-4, SHIMADZU-SPD-20A, Phenomenex Lux, Cellulose-4, Amchemteq AC1 Am-1 with different dimensions and diameter.

Columns were eluted with two mobile phases (Phase A and Phase B) with gradient from 0 to 100% for both phases. Some examples of phases used but not limited: 0.1% diethylamine in MeOH, water (0.05% TFA), MeCN, Hexane (0.1% diethylamine or diisopropylamine), MeOH, dichloromethane, isopropanol, ethanol, MTBE, 0.2% isopropanol in EtOH, 0.1% isopropanol in hexane, 0.1% aqueous diethyl amine, 0.1% or 0.2% 2,6-diethylaniline in tert butyl methyl ether. Peaks were detected at 220 and 254 nm.

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