Campomanesia xanthocarpa Berg. (gabiroba) |
P 1.0 min |
Ascentis RP-Amide (250 × 1 mm, 5 μm) × Ascentis Express C18 (50 × 4.6 mm; 2.7 μm) |
mobile phases: A 0.1% formic acid in water (pH 3) and B 0.1% formic acid in ACN; multi (four-step) segmented gradient: 0-5 min, 2% B; 40 min, 40% B; 50 min, 60% B; 60 min, 100% B; 90 min, 100% B; flow rate 10 µL min-1
|
mobile phase: A 0.1% formic acid in water (pH 3), solvent B 0.1% formic acid in acetonitrile; multi (four-step) segmented gradient 0-40 min 10-16% B; 40-60 min 16-26% B; 60-70 min 30-50%B; 70-105 min 50-90% B; flow rate 2.5 mL min-1
|
DAD; MS |
identification of active polyphenols |
90 |
Two industrial hemps, both were indica dominant hybrid (60% Cannabis indica, 40% Cannabis sativa) strains |
A 0.5 min additional pump: solvent: 0.1% (v/v) formic acid and water, flow rate of 0.020 mL min-1
|
Kinetex PFP (150 × 2.1 mm, 1.7 μm) × Kinetex C18 (50 × 4.6 mm; 2.6 μm) |
mobile phase: A 0.1% formic acid in water; B 0.1% formic acid in methanol; gradient, 0-5 min; 5-8% B, 5-7 min 25% B, 7-18 min 35% B, 18-19 min 40% B, 19-35 min; 55% B, 35-36 min 65% B, 36-52 min 85% B, 52-54 min 100% B, 54-65 min 100% B; flow rate of 0.050 mL min-1
|
mobile phase: A 0.1% formic acid in water; B 0.1% formic acid in acetonitrile; gradient: 0-0.42 min 5-10% B; 10-12 min, 5% B; 12-12.42 min, 10% B; 12.42-33 min, 25% B; 30-33.42 min, 30% B; 33.42-40 min, 25% B; 40-40.42 min, 45% B; 40,42-51 min, 35% B; 51-51.42 min, 70% B; 51.42-60 min, 80% B; and 60-60.42 min, 100% B; flow rate: 2.5 mL min-1
|
DAD; DAD |
µLC × LC separation; a home-made program to do a “demodulation”, which allows discrimination of industrial hemp strains |
91 |
Pistacia vera L. kernel extracts |
P 1.20 min |
Ascentis Express Cyano (150 × 1.0 mm, 2.7 μm) × Ascentis Express C18 (50 × 2.1 mm, 2.7 μm) |
mobile phases: A 0.1% formic acid in water (pH 3), B 0.1% formic acid in ACN; gradient: 0-5 min, 2% B; 5-20 min, 10% B; 20-60 min, 30% B; 60-80 min, 100% B (held for 20 min); flow rate, 15 μL min-1
|
mobile phases: A 0.1% formic acid in water (pH 3) and (B) 0.1% formic acid in ACN; shift gradient: 0-8 min, 1% B; 8-80 min, 1-26 % B; flow rate: 0.8 mL min-1
|
DAD, MS |
polyphenolic fraction of P. vera extracts from diverse geographic origins detected using a shift gradient approach had greater separation space to overcome co-elution issues, resulting in identifying more compounds than conventional one-dimensional LC analysis |
92 |
Olea europeaea L. (olive trees) |
P 0.25 min |
PFP Kinetex F5 column (50 mm × 2.1 mm, 2.6 µm) × Zorbax Eclipse Plus C18 (50 mm × 3 mm, 1.8 µm) |
mobile phases: A 0.05% TFA in water (v/v). B 0.05% TFA in MeOH; gradient: 0-10 min 30% B; 10-25 min 60% B, 25-40 95%, it was kept during 2 min; A re-equilibration step was carried out during 14 min; flow rate: 0.1 mL min-1
|
mobile phases A 0.05% TFA in water (v/v); B 0.05% TFA and ACN; shifted gradient 0-60 min; flow rate: 2.5 mL min-1
|
DAD, DAD |
polyphenolic fingerprints for classification of olive leaves and pulp extracts |
93 |
Bovine serum albumin digest (one protein), yeast-proteome digest (about 6700 proteins) and human kidney-tissue (about 20,000 proteins) |
P |
ZIC-HILIC (200 mm × 200 mm, 5 mm) × C18 (50 mm × 4.6 mm, 3 mm; both columns packed in house |
mobile phases: A 10-mM ammonium formate in water (pH 3). B, 97% ACN: 3% 10 mM ammonium formate, (pH 3); A multi-segment gradient: 0-1 min 95% B 1-2 min, 95-85% B 2-59 min 85-75% B 59-89 75-65% B 89-90 min 65-50% B 90-91 min 95% B equilibration column with 95% B for 30 min; flow rate 1 µL min-1
|
mobile phases: A, 0.1% formic acid in water with 2% ACN B, 0.1% formic acid in 20% water and 80% ACN; gradient: 5% B to 60% B, gradient time was set equal to the modulation time minus 1 min; modulation times (5, 10, 15 and 30 min); flow rate 1.2 µL min-1
|
DAD, MS |
use of a C18 trap column to overcome dilution and solvent incompatibility; a 60% increase in peak capacity and a 17-34% increase in the number of identified proteins were achieved for the samples analyzed (2D-yeast-8280 peptides and 2D-kidney tissue-8843 peptides), without increasing the analysis time (2 h) |
94 |
Rat plasma related to depression |
|
SeQuant ZIC-cHILIC column (150 × 2.1 mm, 3 μm) × Kinetex C8 column (150 × 2.1 mm, 2.6 μm) |
mobile phases: A 0.1% formic acid and 5 mM ammonium acetate in water: ACN (95:5) B ACN: water (95:5) with 0.1% formic acid and 5 mM ammonium acetate; gradient: 0-1.5 min 90% B, 1.5-20 min 90-60% B, 20-22 min 60% B, 22.1-40 min 90% B; flow rate 0.4 mL min-1
|
mobile phase: A water; B ACN: isopropanol (60:40) with 5 mM ammonium acetate; gradient; 0-2 min 0-20% B, 2-18 min 20% B, 18-35 min 20-100% B, 35-39.5 100% B; flow rate 0.4 mL min-1
|
DAD, MS |
simultaneous analysis of the metabolome and lipidome; a total of 319 metabolites were determined within 40 min, including organic acids, nucleosides, carbohydrate derivatives, amino acids, lipids, and other organic compounds; 44 depression-related differential metabolites were screened; compared with conventional LC-MS-based methods, the 2D-LC method covered over 99% of features obtained by two conventional methods |
95 |
AQC-derivatized amino acids |
P |
ACQUITY BEH C18 (150 × 1.0 mm, 1.7 μm) × QNAX-ZWIX(+) tandem column setup consisting of a QN-AX (50 × 3.0 mm, 2.7 μm,) column coupled to a ZWIX(+) (50 × 3.0 mm, 2.7 μm) |
mobile phases: A: 0.05% formic acid + 1% MeOH in water; B: 0.05% formic acid in ACN; gradient: 0- 9.33 min 2.5% B 9-33-17.5 min 9% B 17.5-23.33 min 9% B 23.33-29.17 min 13% B 29.17-40.83 min 13% B 40.38 -44.33 min 25% B 44.33-45.50 min 50% B 45.50-46.67 min 50% B 46.67-47.83 min 0% B 47.83-58.33 min 0% B at 150 μL min-1) 58.33-59.50 min 13% B 59.50-60 min 13% B; flow rate: 0.06 mL min-1
|
mobile phases: A: 10 mM ammonium formate + 10 mM formic acid + 0.5% H2O in MeOH; B: 50 mM ammonium formate + 50 mM formic acid + 0.5% H2O in MeOH, gradient: 0-0.2 min 0% B, 0.2-0.5 min 100% B 0.5-1.5 min 100% B 1.5-1.6 min 0% B 1.6-5 min 0% B, flow rate: 2.5 mL min-1; the final LC × LC 2D gradient without initial hold was: 0-0.35 min 0-100% B 0.35-0.83 min 100% B 0.83-0.85 min 0% B 0.85-1 min 0% B, flow rate: 2.5 mL min-1
|
HRMS |
an LC × LC HRMS method with data-independent SWATH detection for untargeted analysis of peptide derived AQC derivatized AA established for simultaneous enantioseparation of all proteinogenic amino acids, including the side chain isomeric analogues of Leu (Ile, aIle, Nle, Tle) and Thr (aThr, Hse) (a total of 25 components), within a total runtime of 60 min (including reequilibration) |
96 |
Honey samples |
A 0.3 min |
CSP-QN-EC (quinine) (100 × 2.1 mm, 5 mm), × C18 (3.3 2.1 mm, 3 μm) |
mobile phases: A: 50 mM ammonium formate (pH 6.30) and B: 50:50 ACN: MeOH; 0-40 min 100% B 40-50 min 100% B; flow rate: 0.3 mL min-1
|
mobile phases: A 50 mM formic acid; B: ACN gradient: 0 0.25 min 0-70% B; flow rate: 3 mL min-1
|
DAD, DAD |
enantiomeric separation of amino acids |
97 |
Plastic-bonded explosive (PBX) 9501 Composition: 94.9 wt.% HMX, 2.5 wt.% Estane® 5703 (poly (ester urethane)), 2.5 wt.% BDNPA/F nitroplasticizer), 0.1 wt.% Irganox 1010 and PBNA (N-phenyl-naphthylamine) |
P 1.6 min |
Zorbax C18-Extended (2.1 mm × 150 mm; 3.5 µm; × PLGel Mixed C (300 mm × 7.5 mm) |
mobile phase: A water and B tetrahydrofuran; gradient: 0-150 min 10-70 % B; 150-240 min 70% B, 240-300 min 70-100% B, 300-360 min 100% B; flow rate, 0.05 mL min-1
|
mobile phases: tetrahydrofuran; flow rate 4.0 mL min-1 for 1.5 min |
DAD; DAD |
a combination of HPLC and SEC techniques can facilitate the analysis while also yielding additional chemical insights. LC × LC analysis can be simplified with the proposed sample preparation approach |
98 |
Acrylate-modified hyaluronic acid (HAM) |
P |
Zorbax RX-C8 100-5 (150 mm × 2.1 mm, 3.5 mm) × PSS SUPREMA linear M column, (50 mm × 20 mm, 10 μm) |
mobile phase: A water; B ACN; gradient: 0-7 min 0% B, 7-8 min 12% B, 8-15 min 12% B, 15-25 min 40% B, 25-28 min 40% B, 28-30 min 0% B 30-45 min 0% B; flow rate 0.5 mL min-1
|
mobile phase: ACN:H2O (40:60 vol%) with 0.02 M ammonium acetate; flow rate: 4.0 mL min-1 for 3.7 min |
ELSD, ELCD |
HAM separation according to chemical composition followed by separation based on molar mass |
99 |