The UV and optical rotations data were obtained on a Shimadzu UV-2700 spectrometer (Shimadzu Co., Ltd., Kyoto, Japan) and Jasco P-1020 automatic polarimeter (JASCO, Tokyo, Japan), respectively. 1H (500 MHz), 13C (125 MHz), and 2D NMR spectra were measured on an Agilent DD2 spectrometer (Agilent Technologies, Waldbronn, Germany). The mass spectra (ESI-MS) were measured under the positive and negative ion modes by a Waters Xevo G2-XS QTof mass spectrometer (Waters, Milford, MA, United States). Column chromatography was performed on silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and on Sephadex LH-20 (Merck). Preparative TLC plates precoated with silica gel GF254 were purchased from Qingdao Marine Chemical Industry Company.
Agilent dd2 spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The Agilent DD2 spectrometer is a laboratory instrument designed for high-performance nuclear magnetic resonance (NMR) spectroscopy. It provides advanced capabilities for the analysis and characterization of chemical samples. The core function of the DD2 spectrometer is to generate a strong magnetic field and detect the electromagnetic signals emitted by the nuclei of atoms within the sample, enabling the identification and quantification of the chemical components present.
Automatically generated - may contain errors
Lab products found in correlation
Lobar lichroprep rp 18, by Merck Group (2 mentions)
Sephadex lh 20, by Merck Group (2 mentions)
Xevo g2 xs qtof mass spectrometer, by Waters Corporation (1 mentions)
Octadecylsilyl ods reversed phase gel, by YMC (1 mentions)
P 1020, by Jasco (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
Thermo scientific ltq orbitrap xl spectrometer, by Thermo Fisher Scientific (1 mentions)
Analytical grade methanol, by Sinopharm (1 mentions)
Ltq orbitrap xl spectrometer, by Thermo Fisher Scientific (1 mentions)
Hplc grade methanol, by Maclin Biochemical Technology (1 mentions)
Simplicity 185 system, by Merck Group (1 mentions)
6 protocols using agilent dd2 spectrometer
1
Comprehensive Analytical Characterization of Natural Products
2
Solid-State NMR Characterization of Molecular Dynamics
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All experiments were acquired on a
600 MHz Agilent DD2 spectrometer (Agilent Technologies) equipped with
a FastMAS probe in the hardware configuration definition configuration. 13C was referenced indirectly to the decision support system
using the peak at 40.48 ppm of adamantane. The recycle delay was set
to 1.5 s for experiments requiring 1H preparation and 0.75
for experiments starting with 2H preparation. The standard
pulse widths were 1.5 μs for 1H and 13C and 2.0 μs for 2H. In rINEPT experiments, all
delay times were set to 1.25 ms. 2H to 13C RESPIRATIONCP experiments were acquired with 1.8 μs hard
pulses and adiabatic ramps of delta ranging from 1000 to 1500 rad/sec
and beta ranging from 3200/2π to 7500/2π Hz. All experiments
were acquired for 20.48 ms in the direct dimension.
600 MHz Agilent DD2 spectrometer (Agilent Technologies) equipped with
a FastMAS probe in the hardware configuration definition configuration. 13C was referenced indirectly to the decision support system
using the peak at 40.48 ppm of adamantane. The recycle delay was set
to 1.5 s for experiments requiring 1H preparation and 0.75
for experiments starting with 2H preparation. The standard
pulse widths were 1.5 μs for 1H and 13C and 2.0 μs for 2H. In rINEPT experiments, all
delay times were set to 1.25 ms. 2H to 13C RESPIRATIONCP experiments were acquired with 1.8 μs hard
pulses and adiabatic ramps of delta ranging from 1000 to 1500 rad/sec
and beta ranging from 3200/2π to 7500/2π Hz. All experiments
were acquired for 20.48 ms in the direct dimension.
3
Comprehensive Characterization of Novel Compounds
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Specific rotation values were recorded on a JASCO P-1020 digital polarimeter (Tokyo, Japan). UV spectra were obtained with a Lambda 35 UV/Vis spectrophotometer (Perkin Elmer, Waltham, United States). Scientific LTQ Orbitrap XL spectrometer (Thermo Scientific, Waltham) was applied to measure the mass spectra of the new compounds. The 1D and 2D NMR spectra were measured with an Agilent DD2 spectrometer (Agilent Technologies, Santa Clara, United States, 500 MHz for 1H and 125 MHz for 13C). Chemical shifts (δ) were referenced to DMSO-d6 at 2.50 for 1H and 39.5 for 13C. Open column chromatography (CC) was performed by silica gel (200–300 mesh, Qingdao Marine Chemical Factory, Qingdao, China), octadecylsilyl (ODS) reversed-phase gel (30–50 μm, YMC CO., LTD., Japan), and Sephadex LH-20 (GE Healthcare, United States). All solvents used were of either analytical grade or filtered prior to use.
4
Characterization of Fungal Metabolites by HPLC-MS
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High-performance liquid chromatography (HPLC) was performed using a Waters ultra-performance liquid chromatography-class system equipped with a C18 column (1.6 μm, 2.1 × 50 mm) and a photodiode array detector. The chromatographic conditions were as follows: mobile phase: 10% methanol (MeOH), 0–5 min; 10%–100% MeOH, 5–35 min; 100% MeOH, 35–45 min; 100%–10% MeOH, 45–50 min; 10% MeOH, 50–60 min; flow rate: 1 ml/min; ultraviolet detection: 235 nm. High-resolution electrospray ionization mass spectrometry (HRESIMS) data were obtained with a Thermo Scientific LTQ Orbitrap XL spectrometer (Thermo Scientific, Waltham, MA, USA). The 1H, 13C, and two-dimensional nuclear magnetic resonance (NMR) spectra were measured using an Agilent DD2 spectrometer (500 and 125 MHz, respectively) (Agilent, Santa Clara, CA, USA). Open column chromatography was performed using silica gel (200−300 mesh, Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep RP-18 (Merck, Darmstadt, Germany), and Sephadex LH-20 (Merck). All solvents used for HPLC, HRESIMS, and NMR analyses were of analytical grade (purchased from Merck, Darmstadt, Germany). The fungal strain, A. arundinis, was previously isolated from fresh leaves of Nicotiana tabacum L., with the GenBank number MK182939 and CGMCC number 14792 (Zhang et al., 2018 (link)).
5
Isolation and Characterization of Bioactive Compounds
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ChCl, aminoethyl alcohol, D-glucose, glycerol, oxalic acid, lactic acid, urea, methanol-d4, QE, 20-hydroxyecdysone, sodium nitrite, and aluminium trichloride (AlCl3) were purchased from Aladdin Industrial Co., Ltd. (Shanghai, China). HPLC-grade methanol and acetonitrile (ACN) were purchased from Shanghai Macklin Biochemical Co., Ltd. (Shanghai, China). Macroporous resins (D101, HPD 600, NKA-9, HPD 400, and AB-8) and analytical-grade methanol were purchased from Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China). Deionized water was obtained using a Unique-R20 purification system (Xiamen RSJ Scientific Instruments Co., Ltd., Xiamen, China).
Nuclear magnetic resonance (NMR) spectra were recorded on an Agilent DD2 spectrometer (500 MHz for 1H and 125 MHz for 13C NMR; Agilent, CA, USA). High-resolution electrospray ionization–tandem mass spectrometry (HRESI-MS) was performed using an LTQ Orbitrap XL spectrometer (Thermo Scientific, MA, USA).
Nuclear magnetic resonance (NMR) spectra were recorded on an Agilent DD2 spectrometer (500 MHz for 1H and 125 MHz for 13C NMR; Agilent, CA, USA). High-resolution electrospray ionization–tandem mass spectrometry (HRESI-MS) was performed using an LTQ Orbitrap XL spectrometer (Thermo Scientific, MA, USA).
6
Spectroscopic Characterization of Compounds
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If not stated otherwise, solvents and reagents were of analytical quality and obtained from VWR International. Consumables were obtained from Sarstedt. Ultrapure water was produced by a Millipore simplicity 185 system. UV/VIS spectroscopic data were recorded on a Hitachi U-2900 spectrophotometer at room temper-ature using a Hellma 10 mm quartz glass cuvette. The samples were dissolved in methanol at a concentration of 0.1 mg/mL, and methanol was used a blank. The UV/Vis spectra are shown in the Supporting Information (Fig. 3S, Supporting Information). Oneand 2-dimensional NMR spectroscopic experiments were carried out using an Agilent DD2 spectrometer (Agilent Technologies, Santa Clara, USA) at 600 MHz ( 1 H) or 150 MHz ( 13 C) at 299 K. Samples were dissolved in methanol-d 4 (≥ 99.8 % D). Chemical shifts (ppm) were referenced to the residual signals of nondeuterated solvent ( 1 H: 4.870 ppm and 3.31 ppm) and the 13 C isotope signal at 49.00 ppm. The 1D and 2D NMR spectra are shown in the Supporting Information (Fig. 6S to 11S, Supporting Information).
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