A sensitive assay for simultaneous determination of plasma concentrations of valganciclovir and its active metabolite ganciclovir by LC/MS/MS

Abstract This assay allows simultaneous determination of the enantiomers of both disopyramide and its active metabolite, mono-N-dealkyldisopyramide, in 1 mL of plasma or 0.1 mL of urine within approximately 35 min by HPLC with a chiral cellulose-derivative column and ultraviolet detection. Recoveries for the analytes and the internal standard (racemic verapamil) with an extraction from alkalinized plasma or urine into diethyl ether were greater than 90%. Intra- and interassay CVs for disopyramide enantiomers were less than 5.5% at 2.5 mg/L in plasma and less than 6.5% at 25 mg/L in urine; for mono-N-dealkyldisopyramide enantiomers they were less than 6.3% and less than 8.9%, respectively. Intra- and interassay relative errors for determining these analytes in plasma and urine at 2.5 and 25 mg/L, respectively, ranged from -5.9% to +2.5%. The calibration curves for the respective analytes were linear (r = 0.995 or greater, P less than 0.01) from 0.025 to 5.0 mg/L in plasma and from 0.5 to 10 mg/L in urine. The lower detection limits (signal-to-noise ratio of 3) for S(+)-disopyramide and the other analytes were 0.010 and 0.025 mg/L, respectively. We evaluated clinical applicability of this method by determining steady-state plasma concentrations and urinary excretions of the respective analytes in a pediatric patient being treated with racemic disopyramide.

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Validation of an HPLC–MS/MS Method for the Determination of Plasma Ticagrelor and Its Active Metabolite Useful for Research and Clinical Practice

Molecules ◽

10.3390/molecules26020278 ◽

2021 ◽

Vol 26 (2) ◽

pp. 278

Author(s):

Jennifer Lagoutte-Renosi ◽

Bernard Royer ◽

Vahideh Rabani ◽

Siamak Davani

Keyword(s):

Active Metabolite ◽

Plasma Concentrations ◽

Antiplatelet Agent ◽

High Plasma ◽

Therapeutic Drug ◽

Routine Practice ◽

Daily Routine ◽

Limit Of Quantification ◽

Wide Range

Ticagrelor is an antiplatelet agent which is extensively metabolized in an active metabolite: AR-C124910XX. Ticagrelor antagonizes P2Y12 receptors, but recently, this effect on the central nervous system has been linked to the development of dyspnea. Ticagrelor-related dyspnea has been linked to persistently high plasma concentrations of ticagrelor. Therefore, there is a need to develop a simple, rapid, and sensitive method for simultaneous determination of ticagrelor and its active metabolite in human plasma to further investigate the link between concentrations of ticagrelor, its active metabolite, and side effects in routine practice. We present here a new method of quantifying both molecules, suitable for routine practice, validated according to the latest Food and Drug Administration (FDA) guidelines, with a good accuracy and precision (<15% respectively), except for the lower limit of quantification (<20%). We further describe its successful application to plasma samples for a population pharmacokinetics study. The simplicity and rapidity, the wide range of the calibration curve (2–5000 µg/L for ticagrelor and its metabolite), and high throughput make a broad spectrum of applications possible for our method, which can easily be implemented for research, or in daily routine practice such as therapeutic drug monitoring to prevent overdosage and occurrence of adverse events in patients.

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Simultaneous determination of indapamide, perindopril and its active metabolite perindoprilat in human plasma using UPLC-MS/MS method

Journal of Chromatography B ◽

10.1016/j.jchromb.2021.122585 ◽

2021 ◽

Vol 1169 ◽

pp. 122585

Author(s):

Xin Zheng ◽

Huitao Gao ◽

Xinge Cui ◽

Yanbao Zhang ◽

Rui Chen ◽

...

Keyword(s):

Simultaneous Determination ◽

Human Plasma ◽

Active Metabolite

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Development of an LC-MS/MS method for simultaneous determination of ticagrelor and its active metabolite during concomitant treatment with atorvastatin

Journal of Chromatography B ◽

10.1016/j.jchromb.2018.12.018 ◽

2019 ◽

Vol 1105 ◽

pp. 113-119 ◽

Cited By ~ 3

Author(s):

Dorota Danielak ◽

Patrycja Gorzycka ◽

Łukasz Kruszyna ◽

Marta Karaźniewicz-Łada ◽

Franciszek Główka

Keyword(s):

Simultaneous Determination ◽

Active Metabolite ◽

Concomitant Treatment

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Determination of Residues of Flumequine and 7-Hydroxyflumequine in Edible Sheep Tissues by Liquid Chromatography with Fluorimetric and Ultraviolet Detection

Journal of AOAC International ◽

10.1093/jaoac/81.3.519 ◽

1998 ◽

Vol 81 (3) ◽

pp. 519-527 ◽

Cited By ~ 4

Author(s):

Jean-michel Delmas ◽

Anne-marie Chape ◽

Pascal Sanders

Keyword(s):

Liquid Chromatography ◽

Ethyl Acetate ◽

Simultaneous Determination ◽

Rapid Method ◽

Active Metabolite ◽

Fluorimetric Detection ◽

Ultraviolet Detection ◽

Tissue Extracts ◽

Edible Tissues

abstract A simple, sensitive, and rapid method for simultaneous determination of residues of flumequine and its microbiologically active metabolite 7-hydroxyflumequine in 100 mg sheep edible tissues (muscle, liver, kidney, and fat) by liquid chromatography is reported. After liquid-liquid cleanup with ethyl acetate, tissue extracts were injected onto a Select B column. The 2 compounds were determined by ultraviolet and fluorimetric detection. The method was repeatable and reproducible for flumequine and 7-hydroxyflumequine in muscle, liver, kidney, and fat, with limits of detection below 2 and 3 μg/kg for flumequine and 7-hydroxyflumequine, respectively. Mean recoveries for flumequine were 90 ± 7, 82 ± 7,89 ± 5, and 82 ± 6% in muscle, liver, kidney, and fat, respectively. Mean recoveries for 7-hydroxyflumequine were 91 ± 2, 90 ± 4, 86 ± 3, and 84 ± 4% in muscle, liver, kidney, and fat, respectively.

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