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  1. AU="Vong Sok"
  2. AU="Bhat, Moomin Hussain"
  3. AU="Luo, Yupeng"
  4. AU="Sayed, Ahmed I"
  5. AU="Govindaraman, Loganathan T"
  6. AU="De Baere, Thierry"
  7. AU="Dunne, Jean"
  8. AU="Taj, Shafaq"
  9. AU="Hassan, Ashwaa"
  10. AU=Freudenberger Todd D
  11. AU="Bose, Sarah"
  12. AU=Casanova Jean-Laurent
  13. AU="Ho, Gia-Thien-Thanh"
  14. AU="Shao, Hui"
  15. AU="Xu, Y Jun"
  16. AU="Lee, Hae-Ock"
  17. AU=Loscher Wolfgang
  18. AU="Mariani, Nicholas"
  19. AU=Corominas M
  20. AU="Enderami, Seyed Ehsan"
  21. AU="Vaidya, Ratnaraj"
  22. AU=Kawai Yasuyuki
  23. AU="Hilu, John"
  24. AU="Liu, Hao-Wen"
  25. AU="Sandar, H"
  26. AU="Palumbo, Amelia"
  27. AU=Hoshino Ayuko
  28. AU="Grindle, Tina"
  29. AU="Fathy, Ramie"

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  1. Artikel ; Online: Development and validation of an LC-MS/MS method for determination of hydroxychloroquine, its two metabolites, and azithromycin in EDTA-treated human plasma.

    Vong Sok / Florence Marzan / David Gingrich / Francesca Aweeka / Liusheng Huang

    PLoS ONE, Vol 16, Iss 3, p e

    2021  Band 0247356

    Abstract: Background Hydroxychloroquine (HCQ) and azithromycin (AZM) are antimalarial drugs recently reported to be active against severe acute respiratory syndrome coronavirus- 2 (SARS-CoV-2), which is causing the global COVID-19 pandemic. In an emergency ... ...

    Abstract Background Hydroxychloroquine (HCQ) and azithromycin (AZM) are antimalarial drugs recently reported to be active against severe acute respiratory syndrome coronavirus- 2 (SARS-CoV-2), which is causing the global COVID-19 pandemic. In an emergency response to the pandemic, we aimed to develop a quantitation method for HCQ, its metabolites desethylhydroxychloroquine (DHCQ) and bisdesethylchloroquine (BDCQ), and AZM in human plasma. Methods Liquid chromatography tandem mass spectrometry was used to develop the method. Samples (20 μL) are extracted by solid-phase extraction and injected onto the LC-MS/MS system equipped with a PFP column (2.0 × 50 mm, 3 μm). ESI+ and MRM are used for detection. Ion pairs m/z 336.1→247.1 for HCQ, 308.1→179.1 for DHCQ, 264.1→179.1 for BDCQ, and 749.6→591.6 for AZM are selected for quantification. The ion pairs m/z 342.1→253.1, 314.1→181.1, 270.1→181.1, and 754.6→596.6 are selected for the corresponding deuterated internal standards (IS) HCQ-d4, DHCQ-d4, BDCQ-d4, and AZM-d5. The less abundant IS ions from 37Cl were used to overcome the interference from the analytes. Results Under optimized conditions, retention times are 0.78 min for BDCQ, 0.79 min for DHCQ, 0.92 min for HCQ and 1.87 min for AZM. Total run time is 3.5 min per sample. The calibration ranges are 2-1000 ng/mL for HCQ and AZM, 1-500 ng/mL for DHCQ and 0.5-250 ng/mL for BDCQ; samples above the range are validated for up to 10-fold dilution. Recoveries of the method ranged from 88.9-94.4% for HCQ, 88.6-92.9% for DHCQ, 88.7-90.9% for BDCQ, and 98.6%-102% for AZM. The IS normalized matrix effect were within (100±10) % for all 4 analytes. Blood samples are stable for at least 6 hr at room temperature. Plasma samples are stable for at least 66 hr at room temperature, 38 days at -70°C, and 4 freeze-thaw cycles. Conclusions An LC-MS/MS method for simultaneous quantitation of HCQ, DHCQ, BDCQ, and AZM in human plasma was developed and validated for clinical studies requiring fast turnaround time and small samples volume.
    Schlagwörter Medicine ; R ; Science ; Q
    Thema/Rubrik (Code) 600
    Sprache Englisch
    Erscheinungsdatum 2021-01-01T00:00:00Z
    Verlag Public Library of Science (PLoS)
    Dokumenttyp Artikel ; Online
    Datenquelle BASE - Bielefeld Academic Search Engine (Lebenswissenschaftliche Auswahl)

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  2. Artikel ; Online: Determination of unbound piperaquine in human plasma by ultra-high performance liquid chromatography tandem mass spectrometry

    Liusheng Huang / Vong Sok / Usman Aslam-Mir / Florence Marzan / Meghan Whalen / Philip J. Rosenthal / Francesca Aweeka

    Journal of Chromatography Open, Vol 2, Iss , Pp 100042- (2022)

    2022  

    Abstract: Piperaquine (PQ) is an antimalarial drug that is highly protein-bound. Variation in plasma protein contents may affect the pharmacokinetic (PK) exposure of unbound drug, leading to alteration of clinical outcomes. All published methods for determination ... ...

    Abstract Piperaquine (PQ) is an antimalarial drug that is highly protein-bound. Variation in plasma protein contents may affect the pharmacokinetic (PK) exposure of unbound drug, leading to alteration of clinical outcomes. All published methods for determination of PQ in human plasma measure the total PQ including both bound and unbound PQ to plasma proteins. There is no published method for unbound PQ determination. Here we report an ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for determination of PQ in human plasma filtrate prepared by filtering human plasma through Millipore Microcon® centrifugal filters (10k NMWL). The filter cup had to be treated with 5% benzalkonium chloride to reduce non-specific binding to the filter devices before filtration of plasma samples. Multiple reactions monitoring (MRM) of the ion pairs m/z 535/288 for PQ and m/z 541/294 for the internal standard (IS) was selected for quantification. When electrospray ionization (ESI+) was used, paradoxical matrix effect was observed despite the structure similarity of the deuterated IS: Ion suppression for PQ versus ion enhancement for the PQ-d6, even though they were closely eluted: 0.62 min versus 0.61 min. Separation was achieved on Evo C18 column (50 × 2.1 mm, 1.7 μm, Phenomenex Inc.) eluted with 10 mM NH4OH and MeCN. When atmospheric pressure chemical ionization in positive mode (APCI+) was used for ion source, matrix effect diminished. Separation was achieved on a PFP column (30 × 2.1 mm, 1.7 μm, Waters, Corp.) eluted with aqueous 20 mM ammonium formate 0.14% trifluoroacetic acid (A) and methanol-acetonitrile (4:1, v/v) containing 0.1% trifluoroacetic acid (B) at 0.8 mL/min flow rate in a gradient mode: 30–30–80–80–30–30%B (0–0.1–1.0–1.40–1.41–1.50 min). The retention time was 0.67 min for both PQ and the IS. The method was validated with a linear calibration range from 20 to 5,000 pg/mL and applied to clinical samples.
    Schlagwörter Piperaquine ; UHPLC-MS/MS ; Plasma filtrate ; Plasma ; Unbound ; free ; Analytical chemistry ; QD71-142
    Thema/Rubrik (Code) 540
    Sprache Englisch
    Erscheinungsdatum 2022-11-01T00:00:00Z
    Verlag Elsevier
    Dokumenttyp Artikel ; Online
    Datenquelle BASE - Bielefeld Academic Search Engine (Lebenswissenschaftliche Auswahl)

    Volltext online

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    Fernleihe an ZB MED

    Sie können sich den gewünschten Titel als lokale Nutzerin oder lokaler Nutzer von ZB MED direkt an den Standort Köln schicken lassen.

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