The obtained FGFR4/CMCSPs and NCSPs particles were fully characterized by SEM, EDS, TGA and DSC. SEM image was obtained via Hitachi S-4800 field-emission SEM equipped with an EDS detector operating at 15.0 kV (Tokyo, Japan). TGA and DSC results were obtained by STA 449 F3 Jupiter (Selb, Germany). The HPLC/MS system (Shimadzu Corporation, Kyoto, Japan) included a SPD-M20A diode array detector (DAD) and a TOFMS system. Sample volume of 10 μL was analyzed at a flow rate of 1.0 mL min−1 monitoring at 236 nm for PD. The analytical column was a 150 mm × 4.6 mm, 5 mm C18 column (Shimadzu Corporation, Kyoto, Japan). The according mobile phase is consisted of acetonitrile-water-ethanoic acid (70:30:0.5, v/v/v). ASG and its alkaloids were analyzed by 250 mm × 4.6 mm, 5 mm C18 column (Acchrom Corporation, Liaoning, China) monitoring at 220 nm. Mobile phase A: acetonitrile, Phase B: 0.1% aqueous formic acid; gradient: 0–30 min, 5% A–30% A; 30–40 min, 30% A–30%A.
Hplc ms system
Manufactured by Shimadzu
Sourced in Japan
The HPLC/MS system from Shimadzu is a high-performance liquid chromatography and mass spectrometry combination instrument. It is designed for the separation, identification, and quantification of a wide range of chemical compounds. The system integrates the advanced technologies of both HPLC and mass spectrometry to provide reliable and accurate results for various analytical applications.
Automatically generated - may contain errors
Lab products found in correlation
Spd m20a diode array detector dad, by Shimadzu (1 mentions)
S 4800 field emission sem, by Hitachi (1 mentions)
C18 guard column, by Phenomenex (1 mentions)
Lc 20adxr hplc pumps, by Shimadzu (1 mentions)
Sil 30ac autosampler, by Shimadzu (1 mentions)
Dgu 20a3, by Shimadzu (1 mentions)
Spd m20a, by Shimadzu (1 mentions)
Lcms 2020, by Shimadzu (1 mentions)
Lc 20ad, by Shimadzu (1 mentions)
Cbm 20a, by Shimadzu (1 mentions)
Sil 20ac, by Shimadzu (1 mentions)
3 protocols using hplc ms system
1
Comprehensive Characterization of FGFR4/CMCSP Particles
2
Metabolic Stability Evaluation by HPLC-MS
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Metabolic
stability was tested with S9 fractions from rat liver homogenate.36 (link) Briefly, the test compounds were incubated in
the presence of the cofactor NADPH under aerobic conditions. The metabolic
enzyme reactions were stopped after 30 min by addition of acetonitrile.
Controls were obtained by adding the test compounds to a mixture of
S9 fractions and acetonitrile. In deviation from the published procedure,
the extent of metabolism was evaluated by reversed-phase HPLC with
MS detection. The HPLC/MS system from Shimadzu (Kyoto, Japan) consisted
of two LC-20ADXR HPLC pumps, a SIL-30AC autosampler, and an LCMS-2020
single quad detector. Aliquots of 2 μL were injected onto a
HICHROM ACE 3 C18 column (2.1 mm inside diameter ×
100 mm, particle size 3 μm) (HiChrom, Berkshire, U.K.) protected
with a Phenomenex C18 guard column (3 mm inside diameter
× 4 mm). The autosampler temperature was 10 °C, and the
column oven temperature was set to 20 °C. The mobile phase consisted
of acetonitrile/10 mM aqueous ammonium acetate 10:90 (v/v) adjusted
to pH 5 with formic acid (A) and acetonitrile/10 mM aqueous ammonium
acetate 90:10 (v/v) adjusted to pH 5 with formic acid. The gradient
run was from 10 to 100% of solvent B. The flow rate was 0.3 mL/min.
Detection was performed in the ESI+ or ESI– mode. Samples and
controls of each test compound were processed and analyzed in rapid
succession.
stability was tested with S9 fractions from rat liver homogenate.36 (link) Briefly, the test compounds were incubated in
the presence of the cofactor NADPH under aerobic conditions. The metabolic
enzyme reactions were stopped after 30 min by addition of acetonitrile.
Controls were obtained by adding the test compounds to a mixture of
S9 fractions and acetonitrile. In deviation from the published procedure,
the extent of metabolism was evaluated by reversed-phase HPLC with
MS detection. The HPLC/MS system from Shimadzu (Kyoto, Japan) consisted
of two LC-20ADXR HPLC pumps, a SIL-30AC autosampler, and an LCMS-2020
single quad detector. Aliquots of 2 μL were injected onto a
HICHROM ACE 3 C18 column (2.1 mm inside diameter ×
100 mm, particle size 3 μm) (HiChrom, Berkshire, U.K.) protected
with a Phenomenex C18 guard column (3 mm inside diameter
× 4 mm). The autosampler temperature was 10 °C, and the
column oven temperature was set to 20 °C. The mobile phase consisted
of acetonitrile/10 mM aqueous ammonium acetate 10:90 (v/v) adjusted
to pH 5 with formic acid (A) and acetonitrile/10 mM aqueous ammonium
acetate 90:10 (v/v) adjusted to pH 5 with formic acid. The gradient
run was from 10 to 100% of solvent B. The flow rate was 0.3 mL/min.
Detection was performed in the ESI+ or ESI– mode. Samples and
controls of each test compound were processed and analyzed in rapid
succession.
3
Quantifying PTOX in Plant Extracts by HPLC-MS
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To quantify PTOX and to include information obtained from previous
experiments, extracts were obtained through the chloroformic and modified MD
methods.
The presence of PTOX in the extracts was verified by HPLC-MS (negative mode).
The retention time of the peak, UV absorption spectrum and m/z 413 molecular
ion of the standard PTOX (Sigma) were compared with those recorded for
extracts from the HsTD10 selected HR-line. The HPLC-MS system (Shimadzu,
Tokyo, Japan) was equipped with a system controller CBM-20a, 2
binary pumps LC-20AD, degasser DGU-20A3, autosampler SIL-20AC, column oven
CTO20A, UV-Vis diodes detector SPD-M20A, mass spectrometer (LCMS-2020),
ionization source with electro spray (ESI), software version 5a. Dry gas
(N2): 10 L min-1 was employed. Also, scan m/z 330–440 nm,
nebulizer gas flow 1.54 L min-1 was employed. A Zorbax- Eclipse
Plus 4.8 x 150 mm, 5 μm, RP C-18 column was connected to a guard column. The
injection volume was 10 μL, and a flow of 0.8 mL min-1 at 25°C
was employed. An isocratic elution of the mobile phase consisting of
methanol-acetonitrile-water-acetic acid (20:30:50:0.1) was used.
experiments, extracts were obtained through the chloroformic and modified MD
methods.
The presence of PTOX in the extracts was verified by HPLC-MS (negative mode).
The retention time of the peak, UV absorption spectrum and m/z 413 molecular
ion of the standard PTOX (Sigma) were compared with those recorded for
extracts from the HsTD10 selected HR-line. The HPLC-MS system (Shimadzu,
Tokyo, Japan) was equipped with a system controller CBM-20a, 2
binary pumps LC-20AD, degasser DGU-20A3, autosampler SIL-20AC, column oven
CTO20A, UV-Vis diodes detector SPD-M20A, mass spectrometer (LCMS-2020),
ionization source with electro spray (ESI), software version 5a. Dry gas
(N2): 10 L min-1 was employed. Also, scan m/z 330–440 nm,
nebulizer gas flow 1.54 L min-1 was employed. A Zorbax- Eclipse
Plus 4.8 x 150 mm, 5 μm, RP C-18 column was connected to a guard column. The
injection volume was 10 μL, and a flow of 0.8 mL min-1 at 25°C
was employed. An isocratic elution of the mobile phase consisting of
methanol-acetonitrile-water-acetic acid (20:30:50:0.1) was used.
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