Simultaneous determination of tenofovir alafenamide and its active metabolites tenofovir and tenofovir diphosphate in HBV-infected hepatocyte with a sensitive LC–MS/MS method

2017 ◽  
Vol 146 ◽  
pp. 147-153 ◽  
Author(s):  
Bingchen Ouyang ◽  
Fang Zhou ◽  
Le Zhen ◽  
Ying Peng ◽  
Jianguo Sun ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Active Metabolites ◽  
Infected Hepatocyte ◽  
Tenofovir Alafenamide ◽  
Tenofovir Diphosphate

scholarly journals Direct Injection Liquid Chromatographic Technique for Simultaneous Determination of Two Antihistaminic Drugs and Their Main Metabolites in Serum

2007 ◽  
Vol 90 (2) ◽  
pp. 384-390 ◽  
Author(s):  
Samy Emara ◽  
Alaa El-Gindy ◽  
Mostafa K Mesbah ◽  
Ghada M Hadad
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Chromatographic Technique ◽  
Simple Liquid ◽  
Good Precision ◽  
Active Metabolites ◽  
Serum Samples ◽  
Antihistaminic Drugs ◽  
Liquid Chromatographic

Abstract A very simple liquid chromatographic technique was developed and validated for the simultaneous determination of 2 antihistaminic drugs, loratadine (LT) and terfenadine (TR), and their major active metabolites, desloratadine (DL) and fexofenadine (FX), respectively, in human serum. LT, DL, TR, and FX from directly injected serum samples were enriched on a protein-coated RP8 silica precolumn (10 4.6 mm id) while serum constituents, such as proteins and salts, were eluted to waste. Using an online column-switching system, the drugs and their metabolites were quantitatively transferred and separated on a second analytical column (Shim-pack 5 μm particle size cyanopropyl, 250 × 4.6 mm id) followed by ultraviolet detection at 243 nm for LT and DL and 220 nm for TR and FX. Very good precision, accuracy, and linearity were obtained over the range of 101000 ng/mL for LT and DL, 10500 ng/mL for TR, and 103000 ng/mL for FX in human serum. High extraction recoveries from serum ranging from 96.03 to 98.19, 95.44 to 97.26, 95.61 to 98.17, and 95.60 to 97.89 for LT, DL, TR, and FX, respectively, were obtained.

scholarly journals Development of Simultaneous Determination Method of a Pregnan Steroid with Gestagenic Activity – Gestobutanoil and Two its Metabolites in Rat Serum

2021 ◽  
Vol 10 (2) ◽  
pp. 112-118
Author(s):  
E. S. Stepanova ◽  
L. M. Makarenkova ◽  
S. V. Goryainov ◽  
T. A. Fedotcheva ◽  
N. L. Shimanovsky
Keyword(s):  
Blood Serum ◽  
Simultaneous Determination ◽  
Megestrol Acetate ◽  
Reaction Products ◽  
Active Metabolites ◽  
Rat Serum ◽  
Rat Blood ◽  
Esi Ms ◽  
Pharmacologically Active

Introduction. Gestobutanoil is a synthetic pregnane steroid with gestagenic activity. Gestobutanoil has two pharmacologically active metabolites (AMOL and megestrol acetate). This implies the need for a detailed study of the kinetics of metabolites. It is rational to combine the study of the pharmacokinetics of gestobutanoil and its metabolites (AMOL and megestrol acetate). The simultaneous determination of several analytes in the rats’ serum can be carried out using chromatography-mass-spectrometry.Aim. Development of an analytical method for the simultaneous determination of gestobutanoil and two its metabolites in a biomatrix (rat serum).Materials and methods. The following methods were used to determine gestobutanoyl and two its metabolites in a biological matrix: GC-MS, HPLCESI-MS, HPLC-ESI-MS with derivatization, HPLC-APCI-MS.Results and discussion. When working with GC-MS, the chromatographic peaks of gestobutanoyl, AMOL, and megestrol acetate were strongly blurred and superimposed on each other, which is apparently due to the thermolability of the substances. The GC-MS method was abandoned in favor of HPLC. Analytes were separated by HPLC gradient elution on a C18 column. ESI ionization did not give typical protonated ions of gestobutanoyl and AMOL, and the intense signals of their cationized ions and fragment ions, which were observed in the spectra of AMOL and gestobutanoyl, could not ensure the reproducibility of the spectra, since the conditions of their formation are not suitable for routine analysis. Derivatization of analytes to form oximes and substituted hydrazones did not give the expected reaction products for HPLC-ESI-MS. APCI made it possible to remove intense cationized ions from the spectra of gestobutanoyl and AMOL and to increase the reliability of the method. The HPLCAPCI-MS technique was reproduced on model rat blood serum.Conclusion. An HPLC-MS method was developed for the simultaneous determination of gestobutanoyl, megestrol acetate, and AMOL. The technique was tested on a model rat blood serum containing all three analytes.

Simultaneous determination of lidocaine and its principal metabolites by liquid chromatography on silica gel, with aqueous eluent.

1984 ◽  
Vol 30 (5) ◽  
pp. 637-640 ◽  
Author(s):  
K Kushida ◽  
K Oka ◽  
T Suganuma ◽  
T Ishizaki
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Silica Gel ◽  
High Performance ◽  
Reversed Phase ◽  
Active Metabolites ◽  
Lower Detection ◽  
Pharmacologically Active ◽  
Organic Amines

Abstract We describe the simultaneous determination of lidocaine and its pharmacologically active metabolites, monoethylglycinexylidide and glycinexylidide, in plasma by "high-performance" liquid-chromatography. By use of a bare ( unbonded ) silica gel with aqueous eluents, separations of organic amines such as lidocaine and its metabolites, which are very difficult and have a poor peak symmetry on bonded reversed-phase packings, were easily accomplished with a good peak symmetry. The method is sufficiently precise, sensitive, and specific. Analytical recoveries of all compounds were greater than 90%; CVs for reproducibility were less than 5% for all compounds; the lower detection limits were 0.1 mg/L or less. This method can be used to monitor the concentrations of these compounds in plasma and to prevent the concentration-related side-effect(s).

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