Drx 400 instrument

Manufactured by Bruker

Sourced in Germany

The DRX-400 is a nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It is designed to analyze the molecular structure and properties of chemical compounds through the detection and measurement of nuclear magnetic resonances. The core function of the DRX-400 is to provide high-resolution NMR data for research and analytical applications.

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Lab products found in correlation

343 polarimeter, by PerkinElmer (1 mentions) Maxis 4g instrument, by Bruker (1 mentions) Rp c18 column, by YMC (1 mentions) P 1020 digital polarimeter, by Jasco (1 mentions) Rp c18 ods a, by YMC (1 mentions) Apollo 2, by Bruker (1 mentions) J 715 spectropolarimeter, by Jasco (1 mentions) Uv 1800 spectrophotometer, by Shimadzu (1 mentions) Sephadex lh 20, by Cytiva (1 mentions) 1525 binary hplc pump, by Waters Corporation (1 mentions) Perkin elmer 341 polarimeter, by PerkinElmer (1 mentions) Sephadex lh 20, by GE Healthcare (1 mentions) Silica gel 60, by Qingdao Marine Chemical (1 mentions) Pyris diamond differential scanning calorimeter, by PerkinElmer (1 mentions) Silica gel, by Qingdao Marine Chemical (1 mentions) Drx 500 instrument, by Bruker (1 mentions) Pe2400 elemental analyzer, by PerkinElmer (1 mentions)

9 protocols using drx 400 instrument

Phytochemical Profiling of Medicinal Plants

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For the phytochemical profile analysis, 40 g of dried aerial parts of each plant were separately extracted at room temperature with methanol (3 × 24 h). Then, they were filtered and concentrated to dryness to yield residues of 4.6 g (M. officinalis), 9.6 g (S. fruticosa), 6.0 g (M. piperita), 5.3 g (O. dubium), 3.6 g (T. capitatus), and 5.0 g (S. cypria).
For NMR experiments, a part of each sample (10.0 mg) was dissolved in 600 μL of CD₃OD. One- and two-dimensional NMR spectra were recorded on a Bruker 400 DRX instrument at 300 K. Chemical shifts are given in ppm (δ) and are referenced to the solvent signal at 3.31/49.0 ppm (CD₃OD) for ¹H- and ¹³C-NMR, respectively. COSY (COrrelation SpectroscopΥ) and HSQC (heteronuclear single quantum coherence) experiments were performed using standard Bruker microprograms.

Chrysargyris A., Petrovic J.D., Tomou E.M., Kyriakou K., Xylia P., Kotsoni A., Gkretsi V., Miltiadous P., Skaltsa H., Soković M.D, & Tzortzakis N. (2024). Phytochemical Profiles and Biological Activities of Plant Extracts from Aromatic Plants Cultivated in Cyprus. Biology, 13(1), 45.

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Phytochemical Analysis of Sideritis Species

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Precisely, 2 g of aerial parts of each plant were added in 100 mL boiled water for 5 min, separately [11] . Then, 2 mL of each sample were transferred in pre-weighed vials and were concentrated in a vacuum rotary evaporator at room temperature, yielding 0.5 g (S. cypria) and 0.4 g (S. perfoliata subsp. perfoliata). Distilled water was used as solvent for the infusions, being sure that any additive/impurity will not be included in the samples.
For NMR measurements, each sample was dissolved in 600 µL of CD 3 OD. 1D and 2D NMR spectra were recorded on Bruker 400 DRX instrument at 300 K. Chemical shifts are given in ppm (δ) and are referenced to the solvent signal at 3.31 ppm (CD 3 OD). COSY (COrrelation SpectroscopΥ) experiment was performed using standard Bruker microprograms. Parameters used to obtain (i) 1 H-NMR spectra: ns = 16, rg = 101 and acquisition time = 1 min and 30 s and (ii) COSY spectra: ns = 4, rg = 101 and acquisition time = 19 min and 30 s.

Tomou E., Lytra K., Chrysargyris A., Tzortzakis N., & Skaltsa H. (2021). NMR Fingerprint Comparison of Cultivated Sideritis spp. from Cyprus. Agronomy, 11(8), 1503-1503.

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Structural Elucidation of Desholothurin B Analogs

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A Bruker DRX-400 instrument (Rheinstetten, Germany) was used to record NMR spectra and was equipped with a 3 mm broadband inverse (BBI) probe or a 5 mm dual ¹H/¹³C probe. Standard Bruker pulse sequences were used to record ¹H, ¹³C, DEPT135, DEPT90, and 2D (COSY, HSQC, HMBC, NOESY) NMR spectra. Bruker TopSpin version 4.0.8 for Windows (Billerica, MA, USA) was used to process the NMR data.
Desholothurin B (1): white powder (1.6 mg); ¹H NMR (methanol-d₄); and ¹³C NMR (methanol-d₄): HRMS m/z 803.4250 [M+Na]⁺ (calcd for C₄₁H₆₄O₁₄Na: 803.4194; and m/z 485.3267 (aglycon).
12-epi-Desholothurin B (2): white powder (1.9 mg); ¹H NMR (pyridine-d₅); and ¹³C NMR (pyridine-d₅): HRMS 803.4175 [M+Na]⁺ (calcd for C₄₁H₆₄O₁₄Na: 803.4194; and m/z 485.3256 (aglycon).

Puspitasari Y.E., Tuenter E., Foubert K., Herawati H., Hariati A.M., Aulanni’am A., Pieters L., De Bruyne T, & Hermans N. (2023). Saponin and Fatty Acid Profiling of the Sea Cucumber Holothuria atra, α-Glucosidase Inhibitory Activity and the Identification of a Novel Triterpene Glycoside. Nutrients, 15(4), 1033.

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Structural Characterization of Organic Compounds

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¹H and ¹³C NMR spectra were recorded on a Bruker DRX400 instrument at 400 and 100 MHz respectively. Melting points were measured on a Thomas-Hoover capillary apparatus. Optical rotations were recorded on a Perkin-Elmer 343 polarimeter. Infrared spectra were collected on a Thermo-Nicolet 6700 FTIR. High resolution electrospray ionization/time of flight mass spectra were recorded at the OSU Campus Chemical Instrument Center on a Bruker maXis 4G instrument. TLC was performed on silica gel 60 F₂₅₄ precoated aluminum-backed plates and column “filtration”/chromatography was performed on silica gel 60, 70–230 mesh. Analysis and separation by HPLC was conducted on a Beckman unit (model 127 pump, model 166 detector) using a Zorbax-Sil 4.6 × 250 mm column (4:1 hexane/ethyl acetate at 2 ml/min.) or Zorbax-Sil 9.4 × 250 mm column (3:1 hexane/ethyl acetate at 5 mL/min.) respectively, with monitoring at 265 nm. The 2,3,4,6-tetra-O-benzyl-D-glucopyranose was purchased from Alfa Aesar. The [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), referred to as PdCl₂(dppf), was obtained from Frontier Scientific.

Cavanaugh K.R., Narayanasamy S., Walker J.R., Clagett-Dame M, & Curley RW J.r. (2016). Improved Synthesis of the C-Glucuronide/Glycoside of 4-Hydroxybenzylretinone (4-HBR). Journal of carbohydrate chemistry, 35(5), 249-260.

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Spectroscopic Characterization of Compounds

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1D NMR and 2D NMR spectra were recorded on a Bruker DRX-400 instrument. HRESIMS was carried out on Bruker Daltonics Apex ultra 7.0 T Fourier transform mass spectrometer with an electrospray ionization source (Apollo II, Bruker Daltonics, Bremen, Germany). Optical rotations were measured with a P-1020 digital polarimeter (JASCO Corporation, Tokyo, Japan). CD spectra were measured on a J-715 spectropolarimeter (JASCO Corporation). The UV spectra were recorded on a UV-1800 spectrophotometer (Shimadzu, Japan). Thin-layer chromatography (TLC) plates (5 × 10 cm) were performed on GF254 (Branch of Qingdao Marine Chemical Co. Ltd., Qingdao, China) plates. For column chromatography (CC), RP-C18 (ODS-A, 50 µm, YMC, Kyoto, Japan), silica gel (200–300 mesh, 300–400 mesh, Branch of Qingdao Marine Chemical Co. Ltd., Qingdao, China), and Sephadex LH-20 (GE Healthcare Bio-Science AB, Pittsburgh, PA, USA) were used. The high performance liquid chromatography (HPLC) analysis was performed on a Waters 2695–2998 system (Waters, Milford, CT, USA). Semi-preparative HPLC was run with a P3000 pump (CXTH, Beijing, China) and a UV3000 ultraviolet-visible detector (CXTH, Beijing, China), using a preparative RP-C18 column (5 µm, 20 × 250 mm, YMC, Kyoto, Japan).

Wang W., Liao Y., Tang C., Huang X., Luo Z., Chen J, & Cai P. (2017). Cytotoxic and Antibacterial Compounds from the Coral-Derived Fungus Aspergillus tritici SP2-8-1. Marine Drugs, 15(11), 348.

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Analytical Characterization of Natural Products

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Optical rotations were determined using a Perkin-Elmer 341 polarimeter (PerkinElmer Co., Waltham, MA, USA). Melting points were taken on a SGW X-4 micromelting point apparatus (INESA Physico Optical Instrument Co., Ltd., Shanghai, China) and HRESIMS spectra on an API QSTAR mass spectrometer (Applied Biosystem/MSD Sciex, Concord, ON, Canada). ECD spectra were recorded at 25 °C on a MOS-450/SFM300 spectrophotometer (Bio-logic, Claix, France). The ¹H, ¹³C, and 2D NMR spectra were recorded on a Bruker DRX-400 instrument using TMS as an internal standard. Column chromatography was performed on silica gel 60 (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, China). Preparative HPLC was performed on a Waters 1525 Binary HPLC pump and a Waters 2414 refractive index detector using a YMC-Pack ODS-A column (250 mm × 10 mm I.D.; S-5 μm, 12 nm). For Preparative TLC plates (HSGF254, Jiangyou silicone Development Co., Ltd., Yantai, China), Sephadex LH-20 (GE Healthcare, Uppsala, Sweden) and Develosil ODS (50 μm, Nomura Chemical Co. Ltd., Osaka, Japan) were used.

Li G., Ding W., Wan F, & Li Y. (2016). Two New Clerodane Diterpenes from Tinospora sagittata. Molecules, 21(9), 1250.

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Comprehensive Characterization of Compound

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Melting point was measured on a Pyris Diamond Differential scanning calorimeter (Perkin Elmer, Waltham, UK). UV spectra were recorded on a TU-1901 UV spectrometer (Purkinje General, Bejing, China). IR spectra were collected on a Bruker Equinox 55 FTIR/FTNIR Spectrometer (Billerica, MA, USA). ESIMS data were obtained on an MDS Sciex API 2000 LC/MS/MS system (MDS Sciex, Ottawa, ON, Canada). High resolution (HR)-EIMS data were obtained on a MAT95XP mass spectrometer (Thermo Finnigan, Waltham, MA, USA). ¹H NMR, ¹³C NMR, and heteronuclear multiple bond correlation (HMBC) spectra were recorded on a Bruker DRX-400 instrument using TMS as internal standard. Silica gel (200–300 meshes, Qingdao Marine Chemical Ltd., Qingdao, China) was used for column chromatography.

Liu S., Luo Z.H., Ji G.M., Guo W., Cai J.Z., Fu L.C., Zhou J., Hu Y.J, & Shen X.L. (2019). Cajanolactone A from Cajanus cajan Promoted Osteoblast Differentiation in Human Bone Marrow Mesenchymal Stem Cells via Stimulating Wnt/LRP5/β-Catenin Signaling. Molecules, 24(2), 271.

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Comprehensive NMR and Mass Spectroscopy Protocol

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One-dimensional ¹H, ¹³C, and ¹⁹F NMR spectra as well
as two-dimensional ¹H–¹³C HSQC and ¹H–¹³C HMBC experiments
were acquired on a Bruker DRX-400 instrument (400, 101, and 376 MHz,
respectively), a Bruker DRX-500 instrument (500, 126, and 470 MHz,
respectively) or a Bruker Avance NEO 600 instrument (600 and 151 MHz,
respectively), equipped with a Prodigy broadband gradient cryoprobe
using DMSO-d₆ as a solvent and TMS as
an internal standard. High-resolution mass spectrometry (HRMS) was
performed using a Bruker Daltonik MaXis Impact HD quadrupole time-of-flight
mass spectrometer (positive (POS)/negative (NEG) electrospray ionization
or atmospheric-pressure chemical ionization from the MeCN or MeCN/DMSO
solution, at a flow rate of 180 μL·h^–1 with parameters optimized for small molecule detection based on
a preinstalled method for infusion analysis). Elemental analysis was
performed on a PerkinElmer PE 2400 elemental analyzer. Melting points
were determined in open capillaries using a Stuart SMP3 apparatus.
All solvents and commercially available reactants/reagents were used
as received. Noncommercial starting materials were prepared as described
below or according to the literature procedures.

Gazizov D.A., Gorbunov E.B., Rusinov G.L., Ulomsky E.N, & Charushin V.N. (2020). A New Family of Fused Azolo[1,5-a]pteridines and Azolo[5,1-b]purines. ACS Omega, 5(29), 18226-18233.

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Isolation and Characterization of Compounds

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Four different fractions, obtained by normal phase flash chromatography, were separated by an Agilent 1200 HPLC using a Luna C18 (2) column (250 x 4.6 mm, 5 µm). UV-detection was done at 330 nm. Trapping of the analytes was performed with an online SPE system Prospekt 2 (Spark, Holland). HySphere™ Resin general phase (GP) cartridges (Spark, Holland) were used, after conditioning with methanol and equilibrating with water. To increase the concentration of the compound, the HPLC run was repeated and the same compounds were trapped several times on the same cartridge (multi-trapping). After trapping, the cartridges were dried with N2 and compounds were eluted with CD3CN into an NMR tube (3 mm). 1 H, 13 C-NMR and 2D-NMR ( 1 H-1 H correlation spectroscopy (COSY), 1 H-13 C heteronuclear single quantum coherence (HSQC), 1 H-13 C heteronuclear multiple bond correlation (HMBC)) spectra of the isolated compounds were recorded on a Bruker DRX 400 instrument (Bruker, Rheinstetten, Germany) equipped with a zgradient 5 mm dual probe and a 3 mm broadband inverse probe using standard Bruker pulse sequences. All samples were dissolved in either CD3OD, 99.5% D or CD3CN 99.8% D. Chemical shifts are given in  and coupling constants (J) in Hz.

van Dooren I., Foubert K., Bijttebier S., Breynaert A., Theunis M., Exarchou V., Claeys M., Hermans N., Apers S, & Pieters L. (2018). In vitro gastrointestinal biotransformation and characterization of a Desmodium adscendens decoction: the first step in unravelling its behaviour in the human body. The Journal of pharmacy and pharmacology, 70(10).

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