NMR analyses were performed using a Bruker Avance III 600 MHz spectrometer (Bruker Biospin, Rheinstetten, Germany) (600.23 MHz for 1H, 150.93 MHz for 13C) with samples dissolved in DMSO-d6 (99.8% atom D; VWR International, Leuven, Belgium). NMR spectra were referenced by the residual signal of the solvent (δH 2.500 ppm, δC 39.60 ppm). NMR experiments, including 1H NMR, 13C NMR, COSY, 1H-13C HSQC and 1H-13C HMBC, were performed using the software Topspin3 (Bruker Biospin). The 1D spectra, i.e. 1H NMR and 13C NMR spectra, were zero-filled to four-fold data points prior to the Fourier transformation. Moreover, 1H NMR data were multiplied by the two-parameter double-exponential Lorentz-Gauss function to improve resolution, and line broadening (1 Hz) was applied to the 13C NMR data to improve the signal-to-noise ratio. Chemical shifts are listed in δ-scale and coupling constants in Hz. The digital resolution enabled us to declare values to three (δH) or two (δC) decimal places. ESI-MS spectra were measured with a Micromass LC-MS Platform in MeOH with the addition of HCO2H; HRMS spectra (ESI, APCI, FAB) were measured with an LTQ Orbitrap XL instrument (Thermo Fisher Scientific, Waltham, MA, USA) or with a ZAB-EQ instrument (VG Analytical, Manchester, UK).
Ltq orbitrap xl instrument
Manufactured by Thermo Fisher Scientific
Sourced in United States, Germany
The LTQ Orbitrap XL instrument is a high-performance mass spectrometer designed for advanced analytical applications. It combines the ion trap (LTQ) and Orbitrap technologies to provide high-resolution, accurate mass measurements. The core function of the instrument is to enable precise identification and quantification of a wide range of compounds in complex samples.
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Lab products found in correlation
Silica gel, by Qingdao Haiyang Chemical (3 mentions)
Uv 2401 pc spectrophotometer, by Shimadzu (2 mentions)
Sephadex lh 20, by Merck Group (2 mentions)
Dmso d6, by Avantor (1 mentions)
Topspin 3, by Bruker (1 mentions)
Dpx 400, by Bruker (1 mentions)
Acquity uplc h class, by Waters Corporation (1 mentions)
Sq detector 2 mass spectrometer, by Waters Corporation (1 mentions)
Av 400 nmr spectrometer, by Bruker (1 mentions)
2998 pda detector, by Waters Corporation (1 mentions)
Silica gel 60 rp 18 f254s, by Merck Group (1 mentions)
Ascend 700 mhz spectrometer, by Bruker (1 mentions)
Lc 8a, by Shimadzu (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Sephadex lh 20 gel, by Cytiva (1 mentions)
Ods a column, by Shimadzu (1 mentions)
Spd 20a, by Shimadzu (1 mentions)
Avance 600 spectrometer, by Bruker (1 mentions)
Easy nlc 1000 system, by Thermo Fisher Scientific (1 mentions)
18 protocols using ltq orbitrap xl instrument
1
NMR and Mass Spectrometric Analysis of Chemical Compounds
2
Characterization of Organic Compounds
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Chemicals, reagents and analytical grade solvents were purchased from Sigma-Aldrich (Gillingham, UK) unless specified. All reactions were carried out under argon. 1H and 13C NMR spectra were recorded in deuterated dimethyl sulfoxide (DMSO-d6) using a Bruker DPX 400 (400 MHz) spectrometer where chemical shifts (δ) were reported as parts per million (ppm) relative to tetramethylsilane (TMS) as internal standard. Coupling constants (J) are reported in Hertz (Hz) and multiplicities are reported as follows: s (singlet), d (doublet), t (triplet), or m (multiplet). Infrared spectra were recorded on a Perkin Elmer precisely spectrum 100 FT-IR spectrometer. Mass spectrometry data were recorded on a Thermo Fisher LTQ Orbitrap XL instrument. CHN elemental analyses for metal compounds were obtained from MEDAC LTD (Woking, UK), analytical and consultancy services.
3
Analytical Characterization of Natural Products
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Specific rotations were obtained on a WYA-2S digital Abbe refractometer (Shanghai Physico-optical Instrument Factory, Shanghai, China). UV spectra were determined using a Shimadzu UV-2401 PC spectrophotometer (Shimadzu Corporation, Tokyo, Japan), while CD spectra were measured on a JASCO J-715 spectra polarimeter (Japan Spectroscopic, Tokyo, Japan). 1H, 13C and 2D NMR spectra were recorded on a Bruker AV 400 NMR spectrometer using TMS as an internal standard. High-resolution ESI-MS were performed on an LTQ Orbitrap XL instrument (Thermo Fisher Scientific, Bremen, Germany) using peak matching. TLC and column chromatography (CC) were carried out over silica gel (200–400 mesh, Qingdao Marine Chemical Inc., Qingdao, China), or a Sephadex-LH-20 (18−110 µm, Merck, Darmstadt, Germany), respectively. UPLC analysis (Waters Corporation, Milford, MA, USA) was recorded using a Waters system equipped in ESI mode on an Acquity UPLC H-Class connected to an SQ Detector 2 mass spectrometer using a BEH RP C18 column (2.1 × 50 mm, 1.7 µm, 0.5 mL/min). Semi-preparative HPLC was performed using a Waters equipped with a 2998 PDA detector (Waters Corporation, Milford, MA, USA) and a RP C18 column (YMC-Pack ODS-A, 10 × 250 mm, 5 μm, 3 mL/min).
4
Isolation and Characterization of Persicaria senticosa
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Persicaria senticosa was collected from Seo-myeon, Chuncheon-si, Gangwon-do, Korea, in 2016 (GPS: N 37° 55′ 30.1″, E 127° 37′ 57.0″, altitude: 434 m). Voucher specimens (G071) were authenticated by Dr. Chun Whan Choi. Persicaria senticosa were deposited at the herbarium of Biocenter, Gyeonggido Business & Science Accelerator, Suwon, South Korea (Fig.S3 ). The 99.9% methanol extract of thirty-four Polygonum was obtained from the Korea Plant Extract Bank at the Korea Research Institute of Bioscience and Biotechnology (Daejeon, Korea). 1H and 13C NMR experiments were performed on a Bruker Ascend 700 MHz spectrometer with tetramethylsilane (TMS). LC-ESI-MS was obtained on a Triple TOF 5600+ instrument (AB SCIX, USA) and HRESI-MS on a LTQ Orbitrap XL instrument (Thermo, USA). Thin-layer chromatography (TLC) was conducted on Silica gel 60 F254 (Merck, Germany) and Silica gel 60 RP-18 F254S (Merck, Germany) plates. Column chromatography(CC) was performed using Silica gel 60 (70~230 mesh, Merck, Germany), ODS-A (12 nm S-7 μm, YMC GEL, Japan), and preparative HPLC was performed on LC-8A (Shimadzu, Japan).
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Persicaria senticosa was collected from Seo-myeon, Chuncheon-si, Gangwon-do, Korea, in 2016 (GPS: N 37° 55′ 30.1″, E 127° 37′ 57.0″, altitude: 434 m). Voucher specimens (G071) were authenticated by Dr. Chun Whan Choi. Persicaria senticosa were deposited at the herbarium of Biocenter, Gyeonggido Business & Science Accelerator, Suwon, South Korea (Fig.
5
High-resolution LC-MS/MS of Derivatized Octasaccharides
6
NMR and Mass Spectrometry Characterization
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1H and 13C NMR spectra were recorded on a Bruker Avance 600 spectrometer (Bruker, Germany) at 600 (1H) and 150 (13C) MHz, respectively. High-resolution ESI-MS mass spectra were carried out on a LTQ-Orbitrap XL instrument (Thermo, USA). Semi-preparative HPLC was performed on a Shimadzu SPD-20A instrument (Shimadzu, Japan), using an YMC-Pack ODS-A column (250 × 10 mm, 5 µm). Silica gel (200–300 mesh, Haiyang Co., Qingdao, China), and Sephadex LH-20 gel (Amersham Biosciences, USA) were used for column chromatography. Pre-coated silica GF254 plates (Haiyang Co., Qingdao, China) were used for TLC analysis.
7
Comparative Proteomic Analysis of LRIG2 Transgenic Skin
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For mass spectrometry analysis reduced (8% BME) and non‐reduced protein samples of LRIG2‐TG back skin and controls were separated by SDS/PAGE. Gels were stained with Coomassie Brilliant Blue R, and protein bands above 300 kDa were excised. To reduce disulfide bonds, the gel slices were incubated in 45 mm dithioerythritol/50 mm NH4HCO3 for 30 min at 55 °C. Free sulfhydryl groups were blocked using 0.1 m iodoacetamide in 50 mm NH4HCO3 at room temperature for 2 × 15 min. For digestion, gel pieces were minced and covered with 100 ng porcine trypsin in 50 mm NH4HCO3 (Promega, Madison, WI, USA). Peptides were separated on a C18 column (PepMap RSLC, C18, 2 µm, 100A, 75 µm × 50 cm; Thermo Scientific, Rockford, IL, USA) at a flow rate of 200 nL·min−1 using an EASY‐nLC 1000 system (Thermo Scientific, Rockford, IL, USA). The gradients consisted of a 120 min ramp from 2% to 25% B (100% acetonitrile, 0.1% formic acid) and a consecutive ramp to 50% B within 10 min. Mass spectra were acquired using a top 5 data‐dependent method on an online coupled LTQ Orbitrap XL instrument (Thermo Scientific, Rockford, IL, USA). Spectra were searched using mascot V2.4 (Matrix Science Ltd, London, UK) and the murine subset of the UniProt database. For evaluation of the data, scaffold V 4.1 (Proteome Software, Inc, Portland, OR, USA) was used.
8
Offline and Online Mass Spectrometry
9
Synthesis and Characterization of Indole Derivatives
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Indole and its derivatives were purchased from Sinopharm Chemical Reagent Co., Meryer, Acros, Alfa Aesar, and TCI, and were used without further purification. β-(E)-Styrene sulfonyl chlorides and their derivatives were prepared according to literature procedures.9 (link) Melting points were determined in open glass capillaries using a Stuart SMP3 (UK) melting point apparatus and are uncorrected.
1H and 13C NMR spectra were recorded using a Bruker AC-400 FT spectrometer (400 MHz and 100 MHz, respectively) using TMS as an internal standard. NMR multiplicities are abbreviated as follows: s = singlet, d = doublet, dd = double doublet, t = triplet, m = multiplet, q = quartet, br = broad signal. Chemical shifts (δ) were recorded using an LC-TOF spectrometer (Micromass). Electron spray ionization (ESI) mass spectrometry data are expressed in ppm, while coupling constants (J) are expressed in Hz. High resolution mass spectra (HRMS) were obtained using a Thermo LTQ Orbitrap XL instrument equipped with an ESI source and controlled by the software Xcalibur. Elemental analyses were conducted using a LECO-183 CHNS analyzer.
1H and 13C NMR spectra were recorded using a Bruker AC-400 FT spectrometer (400 MHz and 100 MHz, respectively) using TMS as an internal standard. NMR multiplicities are abbreviated as follows: s = singlet, d = doublet, dd = double doublet, t = triplet, m = multiplet, q = quartet, br = broad signal. Chemical shifts (δ) were recorded using an LC-TOF spectrometer (Micromass). Electron spray ionization (ESI) mass spectrometry data are expressed in ppm, while coupling constants (J) are expressed in Hz. High resolution mass spectra (HRMS) were obtained using a Thermo LTQ Orbitrap XL instrument equipped with an ESI source and controlled by the software Xcalibur. Elemental analyses were conducted using a LECO-183 CHNS analyzer.
10
Air- and moisture-sensitive organic synthesis
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All the air- or moisture-sensitive reactions and manipulations were performed under an atmosphere of argon by using standard Schlenk techniques and Drybox (Mikrouna, Supper 1220/750). 1H nuclear magnetic resonance (NMR) and 13C NMR spectra were recorded on a 400- or 500-MHz Bruker Avance spectrometer. CDCl3 was used as solvent. Chemical shifts (δ) were reported in parts per million with tetramethylsilane as the internal standard, and J values were given in hertz. The following abbreviations were used to explain the multiplicities: s, singlet; d, doublet; dd, double of doublets; t, triplet; q, quartet; m, multiplet. Flash column chromatograph was carried out using 200- to 300-mesh silica gel at medium pressure. High-resolution mass spectra (HRMS) were recorded on a liquid chromatography (LC)–time-of-flight spectrometer. Electrospray ionization (ESI)–HRMS data were acquired using a Thermo LTQ Orbitrap XL Instrument equipped with an ESI source. Optical rotation was obtained on a Rudolph Research Analytical (Atopol I). High-performance LC (HPLC) analysis was performed on Agilent 1260 series, and ultraviolet detection was monitored at 230 or 220 nm. Tetrahydrofuran was distilled over sodium. Melting points were measured on a MP-450 (Hanon) melting point apparatus and uncorrected.
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