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Development and Validation of an LC–MS/MS Method for Determination of Tigecycline and Its Epimer in Human Plasma and Its Application in a Pharmacokinetic Study

Wang L., Hu X., Zhu H., Zhang X., Wang C., Han Z.

Acta Chromatographica

2016

Vol. 28, no. 2

239--253

A rapid, selective, sensitive, and simple method for simultaneous determination of tigecycline and its epimer in human plasma samples was developed and validated by liquid chromatography–tandem mass spectrometry (LC–MS/MS). Sample preparation involved one-step protein precipitation by adding 0.1% formic acid–methanol and phosphate buffer (PB) solution to the plasma. Chromatographic separation was obtained with XBridge BEH C18 column (3.5 μm, 50 × 4.6 mm) through a 9.5-min gradient mobile phase at the flow rate of 0.6 mL min−1 at 4 °C. The calibration curves were linear over concentration 5.00–2000 ng mL−1 with correlation coefficient greater than 0.998. Intra-batch and inter-batch accuracy of the assay were in the ranges of −2.90% to 3.00%, and the corresponding precision was less than 6.97%. The extraction recovery of tigecycline and its epimer with the current method were 87.2% and 76.9%, respectively. The applied LC–MS/MS method was shown to be sufficiently sensitive and will be suitable for pharmacokinetic studies.

Synteza idarubicynonu. Inwersja konfiguracji na C-9 w epimerze (9R) syntonu pierścieni AB

Szechner B., Achmatowicz O., Bodalski R., Koszuk J.

Przemysł Chemiczny

2006

T. 85, nr 5

333-337

Opracowano warunki inwersji konfiguracji trzeciorzędowej grupy hydroksylowej w syntonie pierścieni AB idarubicynonu.

Waste 3-acetyl-5,8-dimetoxy-3-hydroxy-3,4-dihydro-2Hnaphthalene-1-spiro-2’-1’-3’-dithiolane 4, a 7:3 mixture of (R) and (S) enantiomers on boiling with ethyl acetate afforded hydroxyketone (R)-4 with high enantiomeric purity (ca. 96%). A two-step inversion of the stereogenic center in the latter gave hydroxyketone (S)-4 in 40% yield. The overall yield of (S)-4, an advanced intermediate in the synthesis of idarubicinone, was thus raised by about 10%.