Lcms 2010

Manufactured by Shimadzu

Sourced in Japan

The LCMS-2010 is a liquid chromatography-mass spectrometry (LC-MS) system manufactured by Shimadzu. It is designed for the analysis of a wide range of chemical compounds. The LCMS-2010 combines liquid chromatography for separation and mass spectrometry for detection and identification of the analytes.

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Lab products found in correlation

Lc 20ab system, by Shimadzu (4 mentions) Luna c18 preparative column, by Shimadzu (4 mentions) Ascend 400 mhz spectrometer, by Bruker (4 mentions) Spd 20a liquid chromatograph, by Shimadzu (3 mentions) Voyager de pro biospectrometry workstation, by Thermo Fisher Scientific (3 mentions) Lc 20adxr pump, by Shimadzu (2 mentions) Sil10 advp, by Shimadzu (2 mentions) Prominence lc 20a instrument, by Shimadzu (2 mentions) Spd 10a uv, by Shimadzu (2 mentions) Spd m20a, by Grace Bio-Labs (2 mentions) Lcms it tof, by Shimadzu (2 mentions) Spd m10avp, by Shimadzu (1 mentions) Luna c18 column, by Shimadzu (1 mentions) Agilent 6530 accurate mass q tof lc ms system, by Agilent Technologies (1 mentions) Jnm al 400 mhz, by JEOL (1 mentions) Uvmini 1240, by Shimadzu (1 mentions) Avance 400 spectrometer, by Bruker (1 mentions) Ppsq 23 protein sequencer, by Shimadzu (1 mentions) Uv 1800 spectrophotometer, by Shimadzu (1 mentions) Esi probe, by Shimadzu (1 mentions)

Spelling variants of this product

LCMS-2010 EV system (11 citations) LCMS-2010 mass spectrometer (8 citations) 2010 LCMS system (7 citations) LCMS-2010 EV Liquid Chromatograph Mass Spectrometer (2 citations) LCMS 2010-A spectrometer (2 citations) LCMS-2010 EV spectrometer (2 citations) LCMS-2010 EV model (2 citations)

31 protocols using lcms 2010

Synthesis of Benzamide Derivative

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Example 105

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A mixture of tert-butyl (3-(((5-((5-(4-(dimethylcarbamoyl)phenyl)pyridin-2-yl)amino)pyridin-2-yl)methyl)carbamoyl)phenyl)carbamate (140 mg, 0.247 mmol) in EtOAc (3 mL) was added HCl/EtOAc (1 M in EtOAc, 5 mL) and the reaction was stirred at 25° C. for 2 h. The yellow solution produced a light yellow solid. TLC showed the reaction was completed. The mixture was concentrated in vacuum. The residue was lyophilized to give 4-(6-((6-((3-aminobenzamido)methyl)pyridin-3-yl)amino)pyridin-3-yl)-N,N-dimethylbenzamide (151 mg, yield: 99%) as a yellow solid. LCMS (Shimadzu LCMS 2010, Mobile phase: from 90% [water+0.04% TFA] and 10% [MeCN+0.02% TFA] to 20% [water+0.04% TFA] and 80% [MeCN+0.02% TFA] in 1.35 min, then under this condition for 0.9 min, finally changed to 90% [water+0.04% TFA] and 10% [MeCN+0.02% TFA] and under this condition for 0.75 min.) purity is 97.02%, Rt=1.592 min; MS Calc'd.: 466.2; MS Found: 467.1 [M+H]⁺. ¹H NMR (400 MHz, DMSO-d₆) δ 2.95 (3H, s), 2.98 (3H, s), 4.78 (2H, d, J=6.0 Hz), 7.16 (1H, d, J=8.8 Hz), 7.48-7.51 (3H, m), 7.59 (1H, t, J=8.0 Hz), 7.76 (2H, d, J=8.4 Hz), 7.81 (1H, s), 7.88 (1H, d, J=9.2 Hz), 7.94 (1H, d, J=8.0 Hz), 8.11 (1H, dd, J=8.8, 2.8 Hz), 8.54 (1H, dd, J=9.2, 2.8 Hz), 8.67 (1H, d, J=2.4 Hz), 9.48 (1H, d, J=3.2 Hz), 9.58 (1H, t, J=4.8 Hz).

US11667651B2. Aminopyridine derivatives as phosphatidylinositol phosphate kinase inhibitors (2023-06-06). HiberCell, Inc. [US]. Inventors: Johan Lindström [SE], Lars Boukharta Persson [SE], Jenny Viklund [SE], Edward A. Kesicki [US], Eugene R. Hickey [US], Markus K. Dahlgren [US], Aleksey I. Gerasyuto [US].

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Synthesis of N-(5-((5-(4-(dimethylcarbamoyl)phenyl)pyridin-2-yl)amino)pyridin-3-yl)nicotinamide

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Example 129

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To a mixture of nicotinic acid (33 mg, 0.27 mmol) in pyridine (2 mL) was added EDC.HCl (52 mg, 0.27 mmol) and 4-(6-((5-aminopyridin-3-yl)amino)pyridin-3-yl)-N,N-dimethylbenzamide (60 mg, 0.18 mmol), the resulting mixture was stirred at 50° C. for 2 h to give a brown solution. LCMS (Rt=0.690 min; MS Calc'd: 438.2; MS Found: 439.1 [M+H]⁺). The mixture was concentrated under reduced pressure to give a residue. The residue was purified by washing with MeOH (5 mL). The filter cake was further purified by prep-HPLC (0.225% FA as an additive) and lyophilized to give N-(5-((5-(4-(dimethylcarbamoyl)phenyl)pyridin-2-yl)amino)pyridin-3-yl)nicotinamide (20.6 mg, yield: 26%) as a white solid. LCMS (Shimadzu LCMS 2010, Mobile phase: from 100% [water+0.04% TFA] to 40% [water+0.04% TFA] and 60% [MeCN+0.02% TFA] in 1.35 min, then under this condition for 0.9 min, finally changed to 100% [water+0.04% TFA] and under this condition for 0.75 min) purity is 100%, Rt=1.452 min; MS Calc'd.: 438.2; MS Found: 439.1 [M+H]⁺. ¹H NMR (400 MHz, DMSO-d₆) δ 2.91-3.05 (6H, m), 7.03 (1H, d, J=8.4 Hz), 7.49 (2H, d, J=8.8 Hz), 7.60-7.64 (1H, m), 7.74 (2H, d, J=8.8 Hz), 8.04 (1H, dd, J=8.4, 2.4 Hz), 8.33-8.37 (1H, m), 8.60 (2H, dd, J=8.0, 2.4 Hz), 8.76-8.78 (1H, m), 8.80 (1H, dd, J=4.8, 1.6 Hz), 8.85-8.88 (1H, m), 9.13-9.17 (1H, m), 9.74 (1H, br s), 10.79 (1H, br s).

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Synthesis of 4-(6-((5-(4-Methoxybenzamido)pyridin-3-yl)amino)pyridin-3-yl)-N,N-Dimethylbenzamide

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Example 142

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To a mixture of 4-(6-((5-aminopyridin-3-yl)amino)pyridin-3-yl)-N,N-dimethylbenzamide (50 mg, 0.15 mmol) in pyridine (2 mL) was added 3-methoxybenzoic acid (34 mg, 0.22 mmol) and EDC.HCl (43 mg, 0.22 mmol), the reaction mixture was stirred at 50° C. for 2 h to give a brown suspension. LCMS (Rt=0.778 min; MS Calc'd: 467.2; MS Found: 468.1 [M+H]⁺). The mixture was concentrated under reduced pressure to give a residue. The residue was purified by washing with MeOH (5 mL) to give a crude product. Then further purified by prep-HPLC (0.05% NH₃.H₂O as an additive) to give 4-(6-((5-(4-methoxybenzamido)pyridin-3-yl)amino)pyridin-3-yl)-N,N-dimethylbenzamide (20.3 mg, yield: 29%) as a pale yellow powder. LCMS (Shimadzu LCMS 2010, Mobile phase: from 100% [water+0.04% TFA] to 40% [water+0.04% TFA] and 60% [MeCN+0.02% TFA] in 1.35 min, then under this condition for 0.9 min, finally changed to 100% [water+0.04% TFA] and under this condition for 0.75 min) purity is 100%, Rt=1.645 min; MS Calc'd: 467.2; MS Found: 468.1 [M+H]⁺. ¹H NMR (400 MHz, DMSO-d₆) δ 2.96-3.05 (6H, m), 3.85 (3H, s), 7.00 (1H, d, J=8.8 Hz), 7.09 (2H, d, J=8.4 Hz), 7.48 (2H, d, J=8.0 Hz), 7.73 (2H, d, J=8.0 Hz), 7.95-8.04 (3H, m), 8.49 (1H, d, J=2.0 Hz), 8.58 (1H, d, J=2.8 Hz), 8.65-8.70 (2H, m), 9.48 (1H, br s), 10.27 (1H, br s).

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HPLC-MS Analysis of Phenolic Compounds

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HSEs were analyzed using a Shimadzu Prominence LC-20A instrument (Shimadzu, Milan, Italy) equipped with two LC-20 AD XR pumps, SIL-10ADvp, CTO-20 AC column oven, and DGU-20 A3 degasser coupled to an SPD-M10Avp PDA detector and a mass spectrometer detector (LCMS-2010, Shimadzu, Tokyo, Japan) equipped with an electrospray (ESI) interface. Separation was performed using a Core Shell column (150 µm, 4.6 mm I.D., 2.7 µm d.p.) (Merck KGaA, Darmstadt, Germany), with the mobile phase composed of 1% aqueous formic acid (A) and acetonitrile (B), pumped at a flow rate of 1 mL/min. Phenolic compound separation was obtained by applying the following gradient: t = 00 0%B; t = 40 30%B; t = 41 100%B; t = 48 100%B; t = 49 0%B; t = 56 0%B. The injection volume was 2 µL. Data were acquired using a PDA in the range 210–400 nm and chromatograms were extracted at 360 nm and at 280 nm. MS-chromatograms were acquired in negative ionization mode, using the following parameters: nebulizing gas flow rate (N2): 1.5 mL min⁻¹; event time: 1 s; mass spectral range: m/z 100–800; scan speed: 1000 amu/s; detector voltage: 1.5 kV; interface temperature: 250 °C; CDL temperature: 300 °C; heat block temperature: 300 °C; interface voltage: −3.50 kV; Q-array voltage: 0.0 V; Q-array RF: 150.0 V.

Spagnuolo L., Della Posta S., Fanali C., Dugo L, & De Gara L. (2023). Chemical Composition of Hazelnut Skin Food Waste and Protective Role against Advanced Glycation End-Products (AGEs) Damage in THP-1-Derived Macrophages. Molecules, 28(6), 2680.

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Preparative HPLC Purification of Compounds

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Individual compounds were purified using preparative HPLC with a dual pump Shimadzu LC-20AB system equipped with a Luna C18 preparative column (21.5 x 150 mm, 5 micron) at λ = 214 nm, with a mobile phase of (A) H₂O (+0.1% formic acid)/(B) acetonitrile (ACN) (+0.1% formic acid) at a flow rate of 15 mL/min; gradients varied by compound based on hydrophobicity. The purities of synthesized compounds were confirmed to be greater than 95% by LC/MS analysis on a Shimadzu LCMS-2010 instrument with ESI Mass Spec and SPD-20A Liquid Chromatograph equipped with a Luna C18 column (50 x 4.6 mm, 5micron) with a mobile phase of (A) H₂O (+0.1% formic acid)/(B) ACN (+0.1% formic acid) (5-95% over 6 min with a 4 min rinse). ¹H NMR spectra were recorded in DMSO-d₆ or Chloroform-d on a Bruker Ascend 400 MHz spectrometer at 400.14 MHz.

Doering S.R., Freeman K., Debevec G., Geer P., Santos R.G., Lavoi T.M., Giulianotti M.A., Pinilla C., Appel J.R., Houghten R.A., Ericson M.D, & Haskell-Luevano C. (2021). Discovery of Nanomolar Melanocortin-3 Receptor (MC3R) Selective Small Molecule Pyrrolidine Bis-Cyclic Guanidine Agonist Compounds Via a High Throughput “Unbiased” Screening Campaign. Journal of medicinal chemistry, 64(9), 5577-5592.

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Characterization of Organic Compounds

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The NMR spectra were recorded using JEOL ECA 600 MHz, JEOL JNM-AL 400 MHz (Jeol, Tokyo, Japan), and Bruker FT 300 MHz (Bruker Biospin GmbH, Karlsruhe, Germany) spectrometer using TMS as an internal standard. Chemical shift (δ) is expressed in ppm with reference to the TMS signals. Low ESI-MS spectra were obtained on a Shimadzu LCMS-2010. High-resolution electrospray ionization mass spectra (HR-ESI-MS) were obtained using an Agilent 6530 Accurate-Mass Q-TOF LC/MS system. The CD spectra were recorded using Jasco J-815 (150-L) (JASCO Crop., Tokyo, Japan). The UV spectra were recorded using UVmini-1240 (Shimadzu, Kyoto, Japan). GC was carried out on a Shimadzu-2010 (Shimadzu, Kyoto, Japan) spectrometer: detector, FID; detection temperature, 300 °C; column, SPB-1 (0.25mm i.d. × 30 m); column temperature, 230 °C; carrier gas, He (2 mL/min) injection temperature, 250 °C; injection volume, 0.5 μL. Column chromatography was performed using silica gel (Kieselgel 60, 70–230 mesh and 230–400 mesh, Merck, Darmstadt, Germany) and C-18 resins (30–50 µm, Fuji Silysia Chemical Ltd., Kasugai, Japan).

Yang S.Y., Lee S.H., Tai B.H., Jang H.D, & Kim Y.H. (2018). Antioxidant and Anti-Osteoporosis Activities of Chemical Constituents of the Stems of Zanthoxylum piperitum. Molecules : A Journal of Synthetic Chemistry and Natural Product Chemistry, 23(2), 457.

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HPLC-ESI-MS Analysis of Organic Compounds

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LC analysis was performed by using a HPLC–electrospray ionization-MS (HPLC–ESI-MS) instrument from Shimadzu (LCMS-2010; Shimadzu, Kyoto, Japan). Chromatographic separation was performed on a reversed-phase HPLC L-column ODS (i.d.: 2.1 mm × 150 mm; particle size: 5 μm; pore size: 12 nm). The mobile phase consisted of 20 mmol/L ammonium acetate (pH 4.5) (mobile phase A) and acetonitrile (mobile phase B). The gradient conditions were as follows: (1) a linear gradient from 20% to 60% mobile phase B (for 15 min) and (2) isocratic elution at 60% mobile phase B (for 5 min). The flow rate was 0.2 mL/min and the injection volume was 5 μL; the column oven was maintained at 40°C. The sample solution for HPLC was injected and analyzed in the ESI (+) mode with selected ion monitoring (SIM) using selected ion masses of m/z 288[PA–Cl], m/z 268[AO–Cl], and m/z 443[RB–Cl–H] for LC/MS detection.

Tatebe C., Zhong X., Ohtsuki T., Kubota H., Sato K, & Akiyama H. (2014). A simple and rapid chromatographic method to determine unauthorized basic colorants (rhodamine B, auramine O, and pararosaniline) in processed foods. Food Science & Nutrition, 2(5), 547-556.

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Spectroscopic Characterization of Organic Compounds

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IR spectra was determined in the KBr pellet using a JASCO FT-IR model 5300 spectrophotometer with polystyrene as reference. NMR spectra were recorded at 400 MHz for ¹H NMR and 100 MHz for ¹³C NMR on Bruker-Avance-400 spectrometer with chloroform-d as solvent and tetramethylsilane (TMS) as reference (δ = 0 ppm) in DMSO-d6 at 25 °C. The chemical shift was expressed in δ, downfield from the signal of internal TMS. Mass spectra were recorded using LC–MS-2010 (Shimadzu).

Kamatham S., Kumar N, & Gudipalli P. (2015). Isolation and characterization of gallic acid and methyl gallate from the seed coats of Givotia rottleriformis Griff. and their anti-proliferative effect on human epidermoid carcinoma A431 cells. Toxicology Reports, 2, 520-529.

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Phenolic Compounds Separation by LC-MS

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The analyses were carried out on a Shimadzu Prominence LC-20A instrument (Shimadzu, Milan, Italy) equipped with two LC-20 AD XR pumps, SIL-10ADvp, CTO-20 AC column oven and DGU-20 A3 degasser coupled to a SPD-M10Avp PDA detector and a mass spectrometer detector (LCMS-2010, Shimadzu, Tokyo, Janpan) equipped with ESI interface. MS data were acquired by Shimadzu LCsolution Ver. 3.7 software (Shimadzu, Tokyo, Janpan). Phenolic compounds separation was carried out using a PFPColumn (150 × 2.1 mm I.D., 2.7 μm d.p.) (Merck KGaA, Darmstadt, Germany). Elution was performed at 40 °C with H₂O/0.1% HCOOH (solvent A) and methanol/acetonitrile at 1:1 (v/v)/0.1% HCOOH (solvent B) at a constant flow–rate of 0.2 mL/min. The gradient elution profile was as follows: 0–5 min 5% B, 5–15 min 5–30% B, 15–40 min 30–50% B, 40–50 min 50–100% B. The injection volume was 2 μL. Data were acquired using a PDA in the range 210–400 nm and the chromatograms were extracted at 280 nm. Chromatograms were acquired in the MS instrument using ESI as interface in negative ionization mode using the following parameters: nebulizing gas flow (N₂): 1.5 mL·min⁻¹; Event time: 1 s; mass spectral range: 100–800 m/z; scan speed: 1000 amu/sec; detector voltage: 1.5 kV; Interface temperature: 250 °C; CDL temperature: 300 °C; heat block: 300 °C; interface voltage: −3.50 kV; Q-array: 0.0 V; Q-array RF: 150.0 V.

Fanali C., Della Posta S., Vilmercati A., Dugo L., Russo M., Petitti T., Mondello L, & de Gara L. (2018). Extraction, Analysis, and Antioxidant Activity Evaluation of Phenolic Compounds in Different Italian Extra-Virgin Olive Oils. Molecules, 23(12), 3249.

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Peptide Cleavage Identification via Mass Spectrometry

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The peptide cleavage sites were identified using mass spectrometry (LCMS-2010 EV Shimadzu, Tokyo, Japan) and/or peptide sequencing, using a PPSQ-23 protein sequencer (Shimadzu, Tokyo, Japan) [16] (link).

Marcondes M.F., Alves F.M., Assis D.M., Hirata I.Y., Juliano L., Oliveira V, & Juliano M.A. (2015). Substrate specificity of mitochondrial intermediate peptidase analysed by a support-bound peptide library. FEBS Open Bio, 5, 429-436.

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