Drug metabolite identification using ultrahigh‐performance liquid chromatography–ultraviolet spectroscopy and parallelized scans on a tribrid Orbitrap mass spectrometer

2020 ◽  
Vol 34 (10) ◽  
Author(s):  
Stephen D. Wilkinson ◽  
Scott Martin ◽  
Alexandra L. Orton ◽  
Roshini Markandu ◽  
Barry C. Jones
Keyword(s):  
Liquid Chromatography ◽  
Mass Spectrometer ◽  
Metabolite Identification ◽  
Ultraviolet Spectroscopy ◽  
Drug Metabolite ◽  
Orbitrap Mass Spectrometer ◽  
Ultrahigh Performance Liquid Chromatography

scholarly journals Styryllactones and Acetogenins from the Fruits of Goniothalamus macrocalyx

2014 ◽  
Vol 9 (4) ◽  
pp. 1934578X1400900 ◽  
Author(s):  
Quy Hung Trieu ◽  
Huong Doan Thi Mai ◽  
Van Cuong Pham ◽  
Marc Litaudon ◽  
Françoise Gueritte ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Cell Lines ◽  
Mass Spectrometer ◽  
Natural Resource ◽  
Absolute Configuration ◽  
Mcf7 Cell ◽  
Crystallographic Analysis ◽  
Kb Cells ◽  
X Ray ◽  
Orbitrap Mass Spectrometer

Two new styryllactones, macrocalactone (1) and 3-deoxycardiobutanolide (2), were isolated from the fruits of Goniothalamus macrocalyx Ban (Annonaceae), together with seven known compounds including four acetogenins, annonacin (3), solamin (4), isoannonacin (5), trans-murisolinone (6), and three other compounds, 7-acetylaltholactone (7), β-caryophyllene-8R,9R-oxide (8) and 2-(2′-hydroxytetracosanoylamino)-octadecane-l,3,4-triol (9). Their structures were determined by spectroscopic and MS analysis. The absolute configuration of I was determined by X-ray crystallographic analysis. The structures of the acetogenins were confirmed by liquid chromatography coupled to a hybrid quadrupole-time of flight mass spectrometer, using post-column lithium infusion. The results were compared with the fragmentation obtained with a hybrid linear trap-orbitrap mass spectrometer. Compound 7 had cytotoxicity against KB, HepG2, Lu, and MCF7 cell lines with IC50 values of 13.1, 23.7, 26.3 and 60.2 μM, respectively, whereas annonacin (3) was selectively active against KB cells (IC50 value of 6.5 μM). The discovery of 3-deoxycardiobutanolide (2) from the fruits of this plant revealed that G. macrocalyx could be a valuable natural resource to obtain this compound as it has been previously reported to have a significant cytotoxicity against different cancer cell lines, especially HL-60 cells.

scholarly journals Screening 89 Pesticides in Fishery Drugs by Ultrahigh Performance Liquid Chromatography Tandem Quadrupole-Orbitrap Mass Spectrometer

Molecules ◽  
2019 ◽  
Vol 24 (18) ◽  
pp. 3375 ◽  
Author(s):  
Shou-Ying Wang ◽  
Cong Kong ◽  
Qing-Ping Chen ◽  
Hui-Juan Yu
Keyword(s):  
Liquid Chromatography ◽  
High Resolution ◽  
Formic Acid ◽  
Mass Spectrometer ◽  
Ammonium Formate ◽  
High Resolution Mass ◽  
Relative Standard ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Tandem Quadrupole ◽  
Resolution Mass

Multiclass screening of drugs with high resolution mass spectrometry is of great interest due to its high time-efficiency and excellent accuracy. A high-scale, fast screening method for pesticides in fishery drugs was established based on ultrahigh performance liquid chromatography tandem quadrupole-Orbitrap high-resolution mass spectrometer. The target compounds - were diluted in methanol and extracted by ultrasonic treatment, and the extracts were diluted with MeOH-water (1:1, v/v) and centrifuged to remove impurities. The chromatographic separation was performed on an Accucore aQ-MS column (100 mm × 2.1 mm, 2.6 μm) with gradient elution using 0.1% formic acid in water (containing 5 mmol/L ammonium formate) and 0.1% formic acid in methanol (containing 5 mmol/L ammonium formate) in Full Scan/dd-MS2 (TopN) scan mode. A screening database, including mass spectrometric and chromatographic information, was established for identification of compounds. The screening detection limits of methods ranged between 1–500 mg/kg, the recoveries of real samples spiked with the concentration of 10 mg/kg and 100 mg/kg standard mixture ranged from 70% to 110% for more than sixty compounds, and the relative standard deviations (RSDs) were less than 20%. The application of this method showed that target pesticides were screened out in 10 samples out of 21 practical samples, in which the banned pesticide chlorpyrifos were detected in 3 out of the 10 samples.

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