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2 protocols using md 4017

1

Detailed Isolation and Characterization Protocol

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Extractions were performed using a sonicator (VWR Ultrasound cleaner, model-USC 1700D). Analytical TLC was carried out with silica gel 60 F254 precoated aluminum sheets (Merck Art. 1.05554). Compounds on TLC were located using a UV lamp and by heating after spraying with acidic anisaldehyde. Silica gel (Fluka 60741, Merck Art. 7734 and 9385) and Sephadex LH-20 were used for column chromatography. Preparative thin layer chromatography (PTLC) was carried out using silica gel 60 F254 precoated glass plates (Merck Art 1.05715). 1H NMR and 13C NMR were recorded on a Bruker DRX500 (500 MHz for 1H and 125 MHz for 13C) or JEOL JMN-AL300 (300 MHz for 1H and 75 MHz for 13C) spectrometer in CD3OD or CDCl3 solution at 20 °C. Optical rotations were measured on a JASCO P-2200 polarimeter. IR spectra were measured on a JASCO FT/IR-460 spectrometer. UV spectra were recorded on a JASCO MD-4017 photo diode array detector. Positive-ion FABMS were obtained on a JEOL JMX-AX505HA spectrometer.
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2

HPAC Analysis of Mycotoxin Compounds

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HPAC was performed with a HSA-coated column (Faisal et al. 2018 (link)). The HPLC system (Jasco, Tokyo, Japan) used for the analysis included an autosampler (AS-4050), a binary pump (PU-4180), and a diode-array detector (MD-4017). A 5-μL volume of samples (ZAN: 200 μmol/L; ZEN, α-ZAL, β-ZAL, and Z14S: 100 μmol/L; Z14G: 50 μmol/L) was driven through a pre-column filter (Waters, Milford, MA, USA) linked to an immobilized HSA-coated HPAC column (Chiralpak® HSA, 50 × 3.0 mm, 5 μm; Daicel, Tokyo, Japan). The isocratic elution was performed with 0.5-mL/min flow rate at room temperature. The mobile phase contained isopropanol (HPLC grade; VWR, Debrecen, Hungary) and 0.01 mol/L pH 7.0 ammonium acetate buffer (15:85 v/v%). Mycotoxins were detected at 235 nm, and chromatograms were evaluated with ChromNAV software.
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