The fermentation filtrate from the coculture of T. asperellum HG1 and B. subtilis Tpb55 was extracted with ethyl acetate (EtOAc) three times and then evaporated under vacuum to obtain the final extract (9.4 g). The extract was separated using a Sephadex LH-20 chromatography column (CC) (CH2Cl2-methanol [MeOH], 1:1 [vol/vol]) after being eluted on a silica gel CC with 10% EtOAc-petroleum ether. It was further purified by HPLC (Waters e2695-2998; Waters, Milford, MA, USA) using MeOH-H2O (75%) with 0.1% trifluoroacetic acid (TFA) to yield DDA (3.2 mg). The DDA structure was identified using 1H and 13C NMR (DD2 500 MHz NMR spectrometer; Agilent Technologies, Santa Clara, CA, USA) and electrospray ionization (ESI) (Micromass Q-TOF spectrometer; Waters) spectra and compared to the literature and the standard compound purchased from Toronto Research Chemicals Inc. (North York, ON, Canada). 1H NMR (dimethyl sulfoxide-d6 [DMSO-d6], 500 MHz) data are as follows: δ 12.16 (s), 7.14 (1H, dd, J = 15.5, 10.0 Hz), 6.22 (1H, dd, J = 15.5, 10.0 Hz), 6.17 to 6.27 (1H, m), 5.78 (1H, d, J = 15.5 Hz), 2.13 (2H, q, J = 7.0 Hz), 1.39 (2H, dt, J = 14.5, 7.5 Hz), 1.23 to 1.30 (4H, m), 0.86 (3H, t, J = 7.0 Hz). 13C NMR (DMSO-d6, 125 MHz) data are as follows: δ 167.7 (C), 144.6 (CH), 144.2 (CH), 128.3 (CH), 120.1 (CH), 32.3 (CH2), 30.9 (CH2), 27.9 (CH2), 21.9 (CH2), 13.9 (CH3); ESIMS m/z 169.11 (M+H)+.
Dd2 500 mhz nmr spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The DD2 500 MHz NMR spectrometer is a laboratory instrument designed for nuclear magnetic resonance spectroscopy. It operates at a frequency of 500 MHz and is capable of performing various NMR experiments for the analysis of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
P 1020 digital polarimeter, by Jasco (6 mentions)
J 815 150s circular dichroism spectrometer, by Jasco (5 mentions)
Ltq orbitrap xl spectrometer, by Thermo Fisher Scientific (4 mentions)
Micromass q tof spectrometer, by Waters Corporation (3 mentions)
Lobar lichroprep rp 18, by Merck Group (3 mentions)
Uv 2700 spectrophotometer, by Shimadzu (3 mentions)
Sephadex lh 20, by Merck Group (3 mentions)
Sephadex lh 20, by Cytiva (3 mentions)
Du 640 spectrophotometer, by Beckman Coulter (3 mentions)
Waters e2695 2998, by Waters Corporation (2 mentions)
1525 system, by Waters Corporation (2 mentions)
Ltq orbitrap mass spectrometer, by Thermo Fisher Scientific (1 mentions)
P 1020 digital, by Jasco (1 mentions)
Agilent series 1290 infinity hplc instrument, by Agilent Technologies (1 mentions)
L 2455 diode array detector, by Hitachi (1 mentions)
L 2000 hplc system, by Hitachi (1 mentions)
L 2455, by Hitachi (1 mentions)
E2695 separation module, by Waters Corporation (1 mentions)
Xevo g2 xs qtof mass spectrometer, by Waters Corporation (1 mentions)
Silica gel, by Qingdao Marine Chemical (1 mentions)
14 protocols using dd2 500 mhz nmr spectrometer
1
Isolation and Characterization of DDA from Coculture
2
Phytochemical Analysis of Natural Products
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Optical rotations were measured on a JASCO P-1020 digital polarimeter (JASCO Corporation, Tokyo, Japan). The IR spectra were recorded on a Nicolet-Nexus-470 spectrometer (Nicolet Corp., Madison, WI, USA). The NMR spectra were recorded on an Agilent DD2 500 MHz NMR spectrometer (500 MHz for 1H and 125 MHz for 13C), using TMS as an internal standard (Agilent Technologies, Santa Clara, CA, USA). The ESI-MS spectra were obtained from a Micromass Q-TOF spectrometer (Waters Corp., Milford, MA, USA). The HPLC-LTQ-Orbitrap-MS analysis was performed on an Agilent series 1290 Infinity HPLC instrument (Agilent, Technologies, Santa Clara, CA, USA), coupled with an LTQ/Orbitrap mass spectrometer (Thermo Scientific, Bremen, Germany) that was equipped with an electrospray (ESI) interface. The semipreparative HPLC was performed using a Hitachi prep-HPLC system that was coupled with a Hitachi L-2455 diode array detector (Hitachi Corp., Tokyo, Japan) and a Kromasil C-18 preparative HPLC column (250 mm × 10 mm, 5 mm) (Eka Nobel, Bohus, Sweden). Silica gel (Qing Dao Hai Yang Chemical Group Co., Qingdao, China; 200–300 mesh) and Sephadex LH-20 (Amersham Biosciences, Inc., Piscataway, NJ, USA) were used for column chromatography. The pre-coated silica gel plates (Yantai Zifu Chemical Group Co., Yantai, China; G60 and F-254) were used for thin-layer chromatography.
3
Isolation and Characterization of DDA from Coculture
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The fermentation filtrate from the coculture of T. asperellum HG1 and B. subtilis Tpb55 was extracted with ethyl acetate (EtOAc) three times and then evaporated under vacuum to obtain the final extract (9.4 g). The extract was separated using a Sephadex LH-20 chromatography column (CC) (CH2Cl2-methanol [MeOH], 1:1 [vol/vol]) after being eluted on a silica gel CC with 10% EtOAc-petroleum ether. It was further purified by HPLC (Waters e2695-2998; Waters, Milford, MA, USA) using MeOH-H2O (75%) with 0.1% trifluoroacetic acid (TFA) to yield DDA (3.2 mg). The DDA structure was identified using 1H and 13C NMR (DD2 500 MHz NMR spectrometer; Agilent Technologies, Santa Clara, CA, USA) and electrospray ionization (ESI) (Micromass Q-TOF spectrometer; Waters) spectra and compared to the literature and the standard compound purchased from Toronto Research Chemicals Inc. (North York, ON, Canada). 1H NMR (dimethyl sulfoxide-d6 [DMSO-d6], 500 MHz) data are as follows: δ 12.16 (s), 7.14 (1H, dd, J = 15.5, 10.0 Hz), 6.22 (1H, dd, J = 15.5, 10.0 Hz), 6.17 to 6.27 (1H, m), 5.78 (1H, d, J = 15.5 Hz), 2.13 (2H, q, J = 7.0 Hz), 1.39 (2H, dt, J = 14.5, 7.5 Hz), 1.23 to 1.30 (4H, m), 0.86 (3H, t, J = 7.0 Hz). 13C NMR (DMSO-d6, 125 MHz) data are as follows: δ 167.7 (C), 144.6 (CH), 144.2 (CH), 128.3 (CH), 120.1 (CH), 32.3 (CH2), 30.9 (CH2), 27.9 (CH2), 21.9 (CH2), 13.9 (CH3); ESIMS m/z 169.11 (M+H)+.
4
Spectroscopic Characterization of Compounds
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Optical rotations were measured on a P-1020 digital polarimeter (Jasco, Tokyo, Japan) and UV spectra were recorded with MeOH on a UV-2700 spectrophotometer (Shimadzu, Kyoto, Japan). The 1H, 13C, and 2D NMR spectra (500 MHz for 1H and 125 MHz for 13C) were acquired using an DD2 500 MHz NMR spectrometer (Agilent, Santa Clara, CA, USA) with TMS as internal standard. HRESIMS spectra were obtained from a LTQ Orbitrap XL spectrometer (Thermo Scientific, Waltham, MA, USA). Analytical HPLC was performed using a UPLC-class system (Waters, Milford, MA, USA) using a C18 column (1.6 μm, 2.1 mm × 50 mm) equipped with a TUV-detector. Column chromatography (CC) was performed with silica gel (100–200 and 200–300 mesh, Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Merck). All the solvents purchased were of analytical grade or HPLC grade.
5
Spectroscopic Analysis of Natural Products
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Optical rotations were measured on a JASCO P-1020 digital polarimeter. UV spectra were recorded on a Beckman DU 640 spectrophotometer. ECD spectra were recorded on a Jasco J-815-150S circular dichroism spectrometer. IR spectra were recorded on a Nicolet-Nexus-470 spectrometer using KBr pellets. 1H, 13C, and 2D NMR spectra were recorded on an Agilent DD2 500 MHz NMR spectrometer (500 MHz for 1H and 125 MHz for 13C), using TMS as an internal standard. The HRESIMS and ESIMS spectra were obtained from a Micromass Q-TOF spectrometer. A semi-preparative HPLC was performed on a Hitachi L-2000 HPLC system coupled with a Hitachi L-2455 photodiode array detector. A Kromasil C18 semi-preparative HPLC column (250 mm × 10 mm, 5 μm) was used. Silica gel (Qing Dao Hai Yang Chemical Group Co.; 200–300 mesh), Sephadex LH-20 (Amersham Biosciences), and octadecylsilyl silica gel (Unicorn; 45–60 μm) were used for column chromatography (CC). Precoated silica gel GF254 plates (Yan Tai Zi Fu Chemical Group Co., Yantai, People's Republic of China) were used for analytical TLC.
6
Spectroscopic Analysis of Natural Compounds
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UV spectra were obtained with a Shimadzu UV-2700 spectrophotometer (Shimadzu Corp., Kyoto, Japan). The optical rotations and ECD spectra were measured with a Jasco P-1020 digital polarimeter and a Jasco J-815-150S circular dichroism spectrometer (JASCO, Easton, MD, USA), respectively. NMR spectra were recorded on an Agilent DD2 500 MHz NMR spectrometer (Agilent Technologies, Waldbronn, Germany) using the residual solvent peak as the internal standard. HRESIMS spectra were obtained on a Waters Xevo G2-XS QTOF mass spectrometer (Waters Corp., Milford, MA, USA). Semipreparative HPLC was performed on a C18 (SunFire®, 10 µm, 19 × 250 mm) column using a Waters e2695 separation module equipped with a 2998 detector. Commercially available silica gel of 200–300 mesh (Qingdao Marine Chemical Co., Shandong, China) was used for open column chromatography.
7
Spectroscopic Characterization of Organic Compounds
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Optical rotations were determined using a Jasco P-1020 digital polarimeter (Jasco, Tokyo, Japan). UV spectra were recorded using a Shimadzu UV-2700 spectrophotometer (Shimadzu, Kyoto, Japan). ECD spectra were obtained with a Jasco J-815-150S circular dichroism spectrometer (Jasco, Inc., Tokyo, Japan). The NMR spectra were recorded using an Agilent DD2 500 MHz NMR spectrometer (500 MHz for 1H and 125 MHz for 13C, Agilent, Santa Clara, CA, USA). HRESIMS data were obtained using an LTQ Orbitrap XL spectrometer (Thermo Scientific, Waltham, MA, USA). Column chromatography was performed using silica gel (200–300 mesh, Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Merck, Darmstadt, Germany).
8
Spectroscopic Characterization of Organic Compounds
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Optical rotations were measured on a P-1020 digital polarimeter (Jasco, Tokyo, Japan). The 1H-, 13C-, and 2D-NMR spectra were acquired using an Agilent DD2 500 MHz NMR spectrometer (500 MHz for 1H and 125 MHz for 13C), with TMS as an internal standard (Agilent, Santa Clara, CA, USA). Analytical HPLC was performed on a Waters UPLC-class system (Waters, Milford, MA, USA), equipped with a TUV-detector, using a C18 column (1.6 μm, 2.1 mm × 50 mm). Column chromatography (CC) was performed using silica gel (100–200, 200–300 mesh, Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Merck) columns. All the solvents used were of analytical grade.
9
Spectroscopic Characterization of Compounds
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Optical rotations were measured on a JASCO P-1020 digital polarimeter. UV spectra were recorded on a Beckman DU 640 spectrophotometer. ECD spectra were obtained on a Jasco J-815-150S circular dichroism spectrometer. IR spectra were recorded on a Nicolet-Nexus-470 spectrometer using KBr pellets. NMR spectra were measured on an Agilent DD2 500 MHz NMR spectrometer (500 MHz for 1H and 125 MHz for 13C), using TMS as an internal standard. The ESIMS and HRESIMS spectra were obtained from a Micromass Q-TOF spectrometer and a Thermo Scientific LTQ Orbitrap XL spectrometer, respectively. The crystallographic data were collected on a Bruker SMART APEX-II CCD diffractometer equipped with graphite monochromatized Cu Kα radiation (λ = 1.54184 Å). Semi-preparative HPLC was performed on a Waters 1525 system coupled with a Waters 2996 photodiode array detector. A Kromasil C18 semi-preparative HPLC column (250 × 10 mm, 5 μm) was used. Silica gel (Qing Dao Hai Yang Chemical Group Co.; 200–300 mesh), Sephadex LH-20 (Amersham Biosciences) and octadecylsilyl silica gel (Unicorn; 45–60 μm) were used for column chromatography. Precoated silica gel GF254 plates (Yantai Zifu Chemical Group Co., Yantai, People's Republic of China) were used for thin-layer chromatography.
10
Comprehensive Analytical Characterization of Chemical Compounds
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Optical rotations were measured on a JASCO P-1020 digital polarimeter. UV spectra were recorded on a Beckman DU 640 spectrophotometer. ECD spectra were obtained on a Jasco J-815-150S circular dichroism spectrometer. IR spectra were recorded on a Nicolet-Nexus-470 spectrometer using KBr pellets. NMR spectra were measured on an Agilent DD2 500 MHz NMR spectrometer (500 MHz for 1H and 125 MHz for 13C), using TMS as an internal standard. The ESIMS and HRESIMS spectra were obtained from a Micromass Q-TOF spectrometer and a Thermo Scientific LTQ Orbitrap XL spectrometer, respectively. The crystallographic data were collected on a Bruker APEX-II CCD diffractometer equipped with graphite monochromatized Cu Kα radiation. Semi-preparative HPLC was performed on a Waters 1525 system coupled with a Waters 2996 photodiode array detector. A Kromasil C18 semi-preparative HPLC column (250 × 10 mm, 5 μm) was used. Silica gel (Qing Dao Hai Yang Chemical Group Co.; 200–300 mesh), Sephadex LH-20 (Amersham Biosciences) and octadecylsilyl Silica gel (Unicorn; 45–60 μm) were used for column chromatography (CC). Precoated Silica gel GF254 plates (Yantai Zifu Chemical Group Co., Yantai, China) were used for thin-layer chromatography.
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