Qualitative analysis of OH was performed by an LCMS-2020 system (Shimadzu, Japan). An InfinityLab Poroshell 120 EC-C18 column of Agilent (4.6 × 100 mm, 2.2 μm) was employed on an LCMS-2020 system (Shimadzu, Japan) for chromatographic separation and MS1 scan of the samples. The column temperature was maintained at 40°C. The mobile phase was composed of water containing 0.1% formic acid (A) and acetonitrile (B) with a flow rate of 0.30 ml/min. The detection wavelength was 238 nm. The elution program was conducted as follows: 0–3 min at 5% B, 3–20 min at 5–70% B, 20–26 min at 70% B, 26–27 min at 70–5% B, and 27–30 min at 5% B. The injection volume was 5 μL (or 10 μL when using UHPLC separately to quantify the main ingredient asperulosidic acid or prepare fingerprints of 19 batches of OH). The MS1 scan range was from 50 to 1,000 m/z using tuning files as default. The analysis of LCMS-2020 was single quadrupole mass spectrometry. The following MS conditions were used: the ESI–mode; nebulizer gas, 3.0 L/min; dry gas, 10.0 L/min; ion source temperature, 250°C; interface temperature, 220°C; DL temperature, 250°C; and heating block temperature, 400°C. The LC-MS scan was operated with the mass range of m/z 100–1,500.
Lcms 2020 system
Manufactured by Shimadzu
Sourced in Japan
The LCMS-2020 system is a liquid chromatography-mass spectrometry (LC-MS) instrument designed for analytical applications. It combines high-performance liquid chromatography (HPLC) with mass spectrometry (MS) to enable the analysis and identification of a wide range of compounds. The system provides accurate mass measurements and sensitive detection for applications in various fields, including pharmaceutical, environmental, and food analysis.
Automatically generated - may contain errors
Lab products found in correlation
Msl 300 spectrometer, by Bruker (6 mentions)
520 melting point apparatus, by Büchi (5 mentions)
Vp hplc system, by Shimadzu (3 mentions)
Kinetex c18 column, by Phenomenex (2 mentions)
Avance 3 700 mhz spectrometer, by Bruker (2 mentions)
Dionex uhplc, by Thermo Fisher Scientific (2 mentions)
Uv vis photo diode array detector, by Thermo Fisher Scientific (2 mentions)
Q exactive benchtop quadrupole orbitrap mass spectrometer, by Thermo Fisher Scientific (2 mentions)
Dionex rslc, by Thermo Fisher Scientific (2 mentions)
Av600 600 mhz spectrometer, by Bruker (2 mentions)
1h 13c 15n triple resonance inverse probe 1.7 mm microprobe, by Bruker (2 mentions)
C1000 thermal cycler, by Bio-Rad (2 mentions)
Spd m20a, by Shimadzu (2 mentions)
Lc 20at pump, by Shimadzu (2 mentions)
Prominence hplc system, by Shimadzu (2 mentions)
Nucleodur c18 gravity column, by Macherey-Nagel (1 mentions)
Analytical hplc system, by Shimadzu (1 mentions)
Chromolith performance rp 18e column, by Merck Group (1 mentions)
Chirascan plus cd spectrometer, by Applied Photophysics (1 mentions)
Analytical balance, by Mettler Toledo (1 mentions)
52 protocols using lcms 2020 system
1
Qualitative LCMS Analysis of Oldenlandia Herb
2
LCMS-Based Glucoside Characterization
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A Shimadzu LCMS-2020 system (Kyoto, Japan)
equipped with a Nucleodur C18 gravity column (3 μm, 110 Å,
150 × 3 mm, Macherey-Nagel, Düren, Germany) was used.
A linear gradient (10 to 85%) of acetonitrile in ammonium acetate
buffer (5 mM, pH 6.67) over 5 min was used. The column was washed
with 10% acetonitrile for 2.5 min. The flow rate was 0.7 mL/min. The
column temperature was 30 °C. A UV detector tuned to 210 and
262 nm was used. Masses were scanned over the range of 150–800
in the positive mode. The masses of mono-glucoside (452.5; [M + H]+, 453.5; [M + Na]+, 475.5; and [M + K]+, 491.5) and bis-glucoside (614; [M + H]+, 615; [M + Na]+, 637.6; and [M + K]+, 653.6) were also analyzed
in the SIM mode. The obtained data are shown in theSupporting Information Figure S5.
equipped with a Nucleodur C18 gravity column (3 μm, 110 Å,
150 × 3 mm, Macherey-Nagel, Düren, Germany) was used.
A linear gradient (10 to 85%) of acetonitrile in ammonium acetate
buffer (5 mM, pH 6.67) over 5 min was used. The column was washed
with 10% acetonitrile for 2.5 min. The flow rate was 0.7 mL/min. The
column temperature was 30 °C. A UV detector tuned to 210 and
262 nm was used. Masses were scanned over the range of 150–800
in the positive mode. The masses of mono-glucoside (452.5; [M + H]+, 453.5; [M + Na]+, 475.5; and [M + K]+, 491.5) and bis-glucoside (614; [M + H]+, 615; [M + Na]+, 637.6; and [M + K]+, 653.6) were also analyzed
in the SIM mode. The obtained data are shown in the
3
Automated Synthesis Using Flow Chemistry System
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Automated synthesis was performed on a Cetoni flow chemistry system (Cetoni GmbH, Korbussen, DE) using two gas-tight borosilicate glass syringes (SGE gas tight 2.5 ml, luer lock, Trajan Scientific), a reaction chip (Chip Type Dean Flow A, 16 × 12.5 mm, DFM-A1, 5 μl), and an 800-μl reaction coil of polytetrafluoroethylene tubing. The flow through the system was directed by three-way solenoid valves (100T3/S116, Bio-Chem Valve Inc., Chrom Tech, Apple Valley, MN, USA). The analysis block consisted of a Rheodyne MRA splitter (MRA100-000, Kinesis, Vernon Hills, IL, USA) coupled with an Advion Expression CMS (Advion, Ithaca, NY, USA) for in-line mass analysis. This equipment used L-216OU pumps from a VWR LaChrom ULTRA HPLC system (Radnor, PA, USA). An analytical HPLC system (Shimadzu, Kyoto, Japan) equipped with an analytical C18 reverse phase column (Macherey-Nagel, Nucleodur C18 HTec; 5 μm, 150 × 3 mm) was used for follow-up sample analysis. Mass signals were recorded using a Shimadzu LCMS-2020 system (Kyoto, Japan). The automated synthesis system was controlled using the QmixElements software supplied by Cetoni on an Aspire X3990 PC (i3 Intel Core 2120 CPU, 8GB, 1066 MHz DDR3 RAM, Windows 7 OS).
4
Metabolite Extraction and LC/MS Analysis
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Prior to the extraction, 200 μM of internal standard ferulic acid or sesamin were added to the samples appointed for quantitative analysis. Metabolites were extracted twice using 1 mL of ethyl acetate, the resulting organic phase was then evaporated under reduced pressure. After evaporation, samples were resuspended in methanol (MeOH, 99.9 % LC/MS grade, Fischer Scientific) for LC/MS analysis.
Both qualitative and quantitative analysis were performed by liquid chromatography coupled with mass spectrometry (LC/MS) measurements on LCMS‐2020 system (Shimadzu, Tokyo, Japan) equipped with a Chromolith® Performance RP‐18e column (100×4.6 mm, Merck). More details are provided in Tables S7 and S8). Samples appointed for quantitative analysis were made in technical and biological duplicate at least.
Both qualitative and quantitative analysis were performed by liquid chromatography coupled with mass spectrometry (LC/MS) measurements on LCMS‐2020 system (Shimadzu, Tokyo, Japan) equipped with a Chromolith® Performance RP‐18e column (100×4.6 mm, Merck). More details are provided in Tables S7 and S8). Samples appointed for quantitative analysis were made in technical and biological duplicate at least.
5
Quantification of Phenolic Compounds
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The quantification of phenolic compounds was carried out on a Shimadzu LCMS-2020 system equipped with a PDM30A detector. Separation was achieved on BEH-C18 (1.7 μm) column, fitted with a suitable guard column. The mobile phase consisted of 0.1% formic acid in water (A) and methanol (B). The column temperature was set at 30°C. Standards and samples were eluted at a flow rate of 0.24 ml/min using a gradient system. Compounds were identified based on retention time, co-injections, and spectral matching with standards that were procured from Sigma Aldrich. The following standards were used: gallic acid (Cat# 147915), chlorogenic acid (Cat# C3878), p-coumaric acid (Cat# C9008), caffeic acid (C0625), and punicalagin A and B (Cat# P0023).
6
HPLC Purification and Characterization of Peptides
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All RP-HPLC analyses and purifications were carried out using Shimadzu Prominence HPLC systems with SPD-20A UV-Vis detectors and LC-20AT solvent delivery units. Ultimate XB-C4 column (Welch, 5 μm, 4.6×250 mm) was used for analysis at a flow rate of 1 ml min−1, to monitor the ligation reaction and analyze the purity of the peptide products. Ultimate XB-C4 or C18 column (Welch, 5 μm, 10×250 mm or 10 μm, 21.2×250 mm) were used to separate the ligation products and crude peptides, respectively, at a flow rate of 4–6 ml min−1. The purified products were characterized by ESI-MS on a Shimadzu LC/MS-2020 system. The CD spectra were obtained on an Applied Photophysics Chirascan-plus CD Spectrometer.
7
Analytical Instrumentation for Pharmaceutical Assay
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Shimadzu LCMS 2020 system consisting of a quaternary pump was operated on ASCII software application. The software on coded communication with the instrument was used for chromatogram conversion and integration, while Excel 2016 was used for regression analysis of the results obtained. A Mettler Toledo analytical balance was used for all weightings (massing) of pharmaceutical standards. pH measurements were taken using a pre-calibrated pH meter. An Ultra-sonicator (Scientech) was employed for the easy dissolution of analytes. The sampling map was created using all sampling point coordinates with the aid of the Google earth pro, 2020 application.
8
LC-MS Analysis of ABN401 Molecular Weight
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To evaluate the molecular weight of ABN401 and its degradation products, LC-MS analysis was conducted using an LCMS 2020 system (Shimadzu, Kyoto, Japan) with two LC-20AD pumps, CTO-20A column oven, SIL-20A autosampler, CBM-20A controller, SPD-20A DAD, and LCMS 2020 single quadruple mass spectrometer. The UV detection wavelength, column, temperature of the column oven, mobile phase composition, and flow rate were the same as the values used for the quantification HPLC method. Mass analysis was conducted using an electrospray ionization (ESI) source that produces ions in the positive ionization mode. The LC-MS spectra were acquired from m/z 50 to 800. The following parameters were used: nebulizing gas flow, 1.5 L/min; drying gas flow, 15 L/min; ESI interface temperature, 350 °C; desolvation line (DL) temperature, 250 °C; heat block temperature, 200 °C; ESI interface voltage, 4.5 kV; and detector voltage, 1.2 kV. Tuning of the mass spectrometer was performed using the auto-tuning function of LabSolutions LC-MS software.
9
Purification and Characterization of Compounds
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Preparative HPLC was carried out on a LC-Forte/R (YMC Co., Tokyo, Japan) with an ultraviolet (UV) detector (YMC Co., Tokyo, Japan) (230 nm) using a Phenomenex Kinetex C18 column (250 × 21.2 mm, 10 µm, Phenomenex, Torrance, CA, USA), whereas the semi-preparative LC system (Gilson Inc, Middleton, WI, USA) was equipped with a refractive index (RI) detector and a Phenomenex Gemini C6-ph column (250 × 10 mm, 5 µm, Phenomenex, Torrance, CA, USA). NMR spectra were recorded on a Bruker AVACE III 400 spectrometer (Bruker, Billerica, MA, USA) (400 and 100 MHz for 1H and 13C, respectively) in acetone-d6. Chemical shifts in the proton and carbon spectra measured in acetone-d6 were reported in reference to residual solvent peaks at 2.05 and 29.9 ppm, respectively. Ultra-high-performance liquid chromatography (UPLC) ESI mass spectrometry was performed on a Shimadzu LCMS-2020 system (Shimadzu, Kyoto, Japan). High-resolution mass spectra were acquired using a JEOL JMS-700 mass spectrometer (JEOL Ltd, Tokyo, Japan) under electron impact or fast atom bombardment (FAB) conditions at the Korea Basic Science Institute.
10
Quantitative Analysis of Linamarin
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Linamarin in the fermented liquid, distilled spirits and distillers’ stillage were analysed using a LC/MS-2020 system (Shimadzu, Kyoto, Japan). Linamarin was separated by a SynergiTM 4 μm Hydro-RP 80 Å column (150 mm × 2.1 mm, Phenomenex Korea Ltd., Seoul, Korea) maintained at 25 °C. 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) were used as the elution solvents. The elution was started with 2% B, maintaining for 5 min; increased to 100% B in 5 min and hold for 3 min; finally decreased to 2% B in 2 min and maintained for 45 min. Each sample was injected at 5 µL and eluted at a flow rate of 0.3 mL/min. The mass spectrometry was carried out in SIM mode, with the monitoring ion of m/z 265 (M+H2O) in positive ion mode. The presence of linamarin in each sample was verified based on the retention time and identical mass compared with an authentic standard.
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