Spectrometers

Manufactured by Agilent Technologies

Spectrometers are analytical instruments used to measure and analyze the spectrum of light or other forms of electromagnetic radiation. They are designed to separate and detect specific wavelengths or frequencies within a range of the electromagnetic spectrum, such as visible light, ultraviolet, or infrared. Spectrometers are widely used in various scientific and industrial applications for the identification, quantification, and characterization of chemical substances and materials.

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Lab products found in correlation

Gct premier high resolution time of flight mass spectrometer, by Waters Corporation (2 mentions) Silica gel 60 f254, by Merck Group (2 mentions) Rf 5301pc fluorescence spectrophotometer, by Shimadzu (1 mentions) 2400c elemental analyzer, by PerkinElmer (1 mentions) Spectrum 100 ftir spectrophotometer, by PerkinElmer (1 mentions) Superdex 75, by GE Healthcare (1 mentions) Lcms it tof mass spectrometer, by Shimadzu (1 mentions) Maldi tof tof mass spectrometer, by Bruker (1 mentions) Ultraflextreme ultrahigh resolution tof lc ms system, by Bruker (1 mentions) P 2000 polarimeter, by Jasco (1 mentions) V 530 spectrophotometer, by Jasco (1 mentions) J 715 spectropolarimeter, by Jasco (1 mentions) Spectrum 100, by PerkinElmer (1 mentions) J 815 spectrometer, by Jasco (1 mentions) 8452a diode array spectrophotometer, by Hewlett-Packard (1 mentions) 6538 ultra high definition accurate mass q tof system, by Agilent Technologies (1 mentions) Uflc system, by Phenomenex (1 mentions) Gemini c18 column, by Phenomenex (1 mentions) Kinetex c18 column, by Phenomenex (1 mentions)

Close spelling variants of this product

500 MHz and 800 MHz NMR spectrometers 400 or 500 MHz spectrometers VMS-600 spectrometers Gemini-300BB 300 MHz FT-NMR spectrometers 500 spectrometers 700-ES series Inductively-Coupled Plasma-Optical Emission Spectrometers (ICP-OES, Inova 750- and 800-MHz spectrometers Unity spectrometers VNMRS 600 MHz FT-NMR spectrometers Agilent 700 Series ICP Optical Emission Spectrometers

10 protocols using spectrometers

Detailed Synthetic Reaction Protocols

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Example 13

Materials and Methods:Unless stated otherwise, reactions were conducted under an atmosphere of N₂using reagent grade solvents. DCM, and toluene were stored over 3 Å molecular sieves. THF was passed over a column of activated alumina. All commercially obtained reagents were used as received. Thin-layer chromatography (TLC) was conducted with E. Merck silica gel 60 F254 pre-coated plates (0.25 mm) and visualized by exposure to UV light (254 nm) or stained with p-anisaldehyde, ninhydrin, or potassium permanganate. Flash column chromatography was performed using normal phase silica gel (60 Å, 0.040-0.063 mm, Geduran). ¹H NMR spectra were recorded on Varian spectrometers (400, 500, or 600 MHz) and are reported relative to deuterated solvent signals. Data for ¹H NMR spectra are reported as follows: chemical shift (δ ppm), multiplicity, coupling constant (Hz) and integration. ¹³C NMR spectra were recorded on Varian spectrometers (100, 125, or 150 MHz). Data for ¹³C NMR spectra are reported in terms of chemical shift (δ ppm). Mass spectra were obtained from the UC Santa Barbara Mass Spectrometry Facility on a (Waters Corp.) GCT Premier high resolution time-of-flight mass spectrometer with a field desorption (FD) source.

US11759526B2. Method and molecules (2023-09-19). MedImmune, LLC [US], The Regents Of The University Of California [US]. Inventors: Ronald James Christie [US], Changshou Gao [US], Andre Henri St. Amant [US], Javier Read de Alaniz [US].

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Synthesis of Crosslinkers and Non-Natural Amino Acids

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Example 2

Crosslinkers and non-natural amino acids (NNAAs) were prepared based on the general design shown in FIG. 2.1.

Materials and Methods: Unless stated otherwise, reactions were conducted under an atmosphere of N₂using reagent grade solvents. DCM, and toluene were stored over 3 Å molecular sieves. THF was passed over a column of activated alumina. All commercially obtained reagents were used as received. Thin-layer chromatography (TLC) was conducted with E. Merck silica gel 60 F254 pre-coated plates (0.25 mm) and visualized by exposure to UV light (254 nm) or stained with p-anisaldehyde, ninhydrin, or potassium permanganate. Flash column chromatography was performed using normal phase silica gel (60 Å, 0.040-0.063 mm, Geduran). ¹H NMR spectra were recorded on Varian spectrometers (400, 500, or 600 MHz) and are reported relative to deuterated solvent signals. Data for ¹H NMR spectra are reported as follows: chemical shift (6 ppm), multiplicity, coupling constant (Hz) and integration. ¹³C NMR spectra were recorded on Varian spectrometers (100, 125, or 150 MHz). Data for ¹³C NMR spectra are reported in terms of chemical shift (6 ppm). Mass spectra were obtained from the UC Santa Barbara Mass Spectrometry Facility on a (Waters Corp.) GCT Premier high-resolution time-of-flight mass spectrometer with a field desorption (FD) source.

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Comprehensive Characterization Methods

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Total commercially available chemicals for synthesis and test were of reagent grade. A Boetius Block apparatus was used for the report of melting points. A PerkinElmer Spectrum 100 FT-IR spectrophotometer was used for the report of Infrared (IR) spectra. A Varian spectrometers was used for the report of ¹H NMR and ¹³C NMR spectra. The measurement of the elemental analyses was carried out on a Perkin-Elmer 2400C Elemental Analyzer. Ultraviolet spectra were recorded on a PerkinElmer Lamber35 UV spectrophotometer. The fluorescence spectra were carried out in a Shimadzu RF-5301PC fluorescence spectrophotometer. A VG ZAB-HS mass spectrometer was used to record EI mass spectra.

Liu Y., Zhao Z., Huo R, & Liu Q. (2019). Two macrocycle-based sensors for anions sensing. Scientific Reports, 9, 502.

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NMR Analysis of Rif1 CRI Fragment

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The Rif1 CRI fragment was ¹⁵N or ¹⁵N/13C labelled by growing cells in M9 minimal medium containing [¹⁵N]ammonium chloride and [¹³C6]glucose as a sole nitrogen/carbon source. The protein was concentrated to 100–330 µM in an NMR buffer (50 mM sodium phosphate, 200 mM NaCl, 1 mM DTT, pH 6.8). To analyse the interactions, the complex of PP1 and ¹⁵N or ¹⁵N/¹³C labelled CRI was purified on a Superdex 75 gel-filtration column (GE Healthcare) in the NMR buffer and concentrated. NMR measurements were performed at 10 °C on Varian spectrometers operating at a ¹H frequency of 600 or 800 MHz. The ¹H-¹⁵N heteronuclear single quantum coherence (HSQC) spectrum of CRI was assigned using a set of triple resonance experiments: HNCO, intra-residue HN(CA)CO, HN(CO)CA, intra-residue HNCA, HN(COCA)CB and intra-residue HNCACB^{54 (link)}.

Sukackaite R., Cornacchia D., Jensen M.R., Mas P.J., Blackledge M., Enervald E., Duan G., Auchynnikava T., Köhn M., Hart D.J, & Buonomo S.B. (2017). Mouse Rif1 is a regulatory subunit of protein phosphatase 1 (PP1). Scientific Reports, 7, 2119.

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Purification and Characterization of Novel Compounds

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Unless otherwise indicated, all reagents and solvents were used without further purification acquired from commercial suppliers. NMR spectra were acquired on Bruker and Varian spectrometers at 600, 400 MHz for ¹H and 150, 100 MHz for ¹³C, respectively. Melting points (m.p., uncorrected) were measured with a Büchi B-540 m.p. apparatus. High-resolution mass spectra (HRMS) were recorded with a Shimadzu LCMS-IT-TOF mass spectrometer equipped with an electrospray ionisation (ESI) source. Routinely, the procedure of reactions was monitored on silica gel by thin-layer chromatography. The purity of the final compounds (>97%) was verified by high-performance liquid chromatography (HPLC) equipped with a UV-diode array detector.

Zhang C., Zhang Y., Lv Y., Guo J., Gao B., Lu Y., Zang A., Zhu X., Zhou T, & Xie Y. (2022). Chromone-based monoamine oxidase B inhibitor with potential iron-chelating activity for the treatment of Alzheimer’s disease. Journal of Enzyme Inhibition and Medicinal Chemistry, 38(1), 100-117.

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Characterization of Purified Compounds

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All compounds are >95% pure
by HPLC. MS data were recorded from a Bruker ultrafleXtreme ultrahigh-resolution
TOF LC-MS system and a matrix-assisted laser desorption/ionization-time-of-flight
(MALDI-TOF)/TOF Mass Spectrometer (Bruker Daltonics). Optical rotations
were determined using a Jasco P-2000 Polarimeter. ¹H and ¹³C NMR spectra were performed on 800 and 200 MHz Varian spectrometers,
respectively. All standard 2D NMR experimental spectra, including
NOESY, HSQC, HMBC, and COSY, were collected at 25 °C.

Cheng A., Liu C., Ye W., Huang D., She W., Liu X., Fung C.P., Xu N., Suen M.C., Ye W., Sung H.H., Williams I.D., Zhu G, & Qian P.Y. (2022). Selective C9orf72 G-Quadruplex-Binding Small Molecules Ameliorate Pathological Signatures of ALS/FTD Models. Journal of Medicinal Chemistry, 65(19), 12825-12837.

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Characterization of Molecular Compounds by Spectroscopy

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A Perkin-Elmer Spectrum 100 Fourier transform infrared (FTIR) spectrometer was employed to record infrared (IR) spectra on a glassy film. UV spectra were measured in CH3OH on a JASCO V-530 spectrophotometer. ECD spectra of 1, 2, 4, 5, 7 and 8 were recorded on a JASCO J-815 spectrometer in CH3OH (c 0.3). The ECD spectra of 3 were recorded with a JASCO J-715 spectropolarimeter, on CH3CN solutions and using a quartz cell with 0.01 cm path-length. ECD measurement parameters were the following: scan speed 100 nm/min; time-constant 0.5 s; bandwidth 1 nm; 4 accumulations. 1 H and 13 C NMR spectra were recorded at 500/125 MHz in CD3OD on Varian spectrometers. The same solvent was used as internal standard. Carbon multiplicities were determined by DEPT spectra (Berger and Braun, 2004 ) DEPT, COSY-45, HSQC, HMBC (Berger and Braun, 2004) , were performed using Varian

Ka S., Masi M., Merindol N., Di Lecce R., Plourde M.B., Seck M., Górecki M., Pescitelli G., Desgagne-Penix I, & Evidente A. (2020). Gigantelline, gigantellinine and gigancrinine, cherylline- and crinine-type alkaloids isolated from Crinum jagus with anti-acetylcholinesterase activity. Phytochemistry, 175.

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Spectroscopic and Chromatographic Characterization of Natural Products

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UV data were recorded on a Hewlett Packard 8452A diode array spectrophotometer. Optical rotation measurements were made on an AUTOPOL^® III automatic polarimeter. The LC-ESIMS analyses were performed on a Shimadzu UFLC system with a quadrupole mass spectrometer using a Phenomenex Kinetex C₁₈ column (3.0 mm × 75 mm, 2.6 μm) and MeCN-H₂O (0.1% HCOOH) gradient solvent system. HRESIMS spectra were measured using an Agilent 6538 Ultra High Definition (UHD) Accurate-Mass Q-TOF system. NMR spectra were obtained on Varian spectrometers (500 MHz and 400 MHz for ¹H, and 100 MHz for ¹³C) using DMSO-d₆ and CDCl₃ as solvents. Column chromatography was conducted using silica gel and HP20SS. HPLC was performed on a Waters System equipped with a 1525 binary HPLC pump coupled to a 2998 PDA detector with a Phenomenex Gemini C₁₈ column (21.2 × 250 mm or 10 × 250 mm, 5 μm particle size).

King J.B., Carter A.C., Dai W., Lee J.W., Kil Y.S., Du L., Helff S.K., Cai S., Huddle B.C, & Cichewicz R.H. (2019). Design and Application of a High-Throughput, High-Content Screening System for Natural Product Inhibitors of the Human Parasite Trichomonas vaginalis. ACS infectious diseases, 5(8), 1456-1470.

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NMR Spectroscopy of Protein Mutants

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NMR spectra were recorded at 25 1C on Varian spectrometers operating at 600 and 800 MHz. NMR spectra were processed with NMRPipe 29 and analyzed using SPARKY. Spectra were recorded in the PFG sensitivity-enhanced mode for quadrature detection in the 15 N indirect dimension with carrier frequencies for 1 H N and 15 N of 4.73 ppm and 120 ppm, respectively. A squared and 601 phase-shifted sine bell window function was applied in all dimensions for apodization. Time domain data were zero-filled to twice the data set size, prior to Fourier transformation.
PRE rates of 15N-labeled OPN mutants C54, C108, C188, C247, C54-C108, C54-C188, C54-C247, C108-C188, C108-C247, C188-C247 and of BASP mutants C3, C92, C136, C205, C3-C92, C3-C136, C3-205, C92-C136, C92-C205, C136-C205 were obtained with three-point measurements as adapted from the approach by Clore and co-workers. 22

Kurzbach D., Vanas A., Flamm A.G., Tarnoczi N., Kontaxis G., Maltar-Strmečki N., Widder K., Hinderberger D, & Konrat R. (2016). Detection of correlated conformational fluctuations in intrinsically disordered proteins through paramagnetic relaxation interference. Physical chemistry chemical physics : PCCP, 18(8).

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Nuclear Magnetic Resonance Protocols

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All reagents were used as received from commercial suppliers. Unless specified, NMR spectra were recorded at 25 °C on Varian spectrometers operating at 300, 400 or 500 MHz ( 1 H NMR) and 75, 100 or 125 MHz ( 13 C{ 1 H} NMR) respectively. Chemical shifts (δ in ppm, coupling constants J in Hz) were referenced to external SiMe 4 ( 1 H, 13 C{ 1 H}). Assignments are based on homo-and hetero-nuclear shift correlation spectroscopy. High-resolution mass spectrometry was carried out with a Micromass/Waters Corp. USA liquid chromatography with an electrospray source. Elemental analyses were performed at UCD Microanalytic Laboratory using an Exeter Analytical CE-440 elemental analyser. Residual solvents were identified by NMR spectroscopy.

Farrell K., Müller-Bunz H, & Albrecht M. (2016). Versatile bonding and coordination modes of ditriazolylidene ligands in rhodium(iii) and iridium(iii) complexes. Dalton transactions (Cambridge, England : 2003), 45(40).

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