scholarly journals Determination of venlafaxine and its active metabolite O-desmethylvenlafaxine in human plasma by HPLC fluorescence

2018 ◽  
Vol 31 (2) ◽  
pp. e000010 ◽  
Author(s):  
Shujuan Shen ◽  
Chen Zhang ◽  
Yemeng Mao
Keyword(s):  
Human Plasma ◽  
Active Metabolite ◽  
Plasma Concentrations ◽  
Regression Equation ◽  
Therapeutic Drug ◽  
Dihydrogen Phosphate ◽  
Simple Method ◽  
Column Temperature ◽  
Clinical Detection

BackgroundTherapeutic drug monitoring guides clinical individualised medication by measuring plasma concentration, which could improve the curative effect, avoid drug overdose and reduce the incidence of adverse reactions. At present, there are few reports on the clinical detection of venlafaxine and its active metabolite O-desmethylvenlafaxine. In this paper, the detection method of venlafaxine and O-desmethylvenlafaxine in blood plasma was established, which provides an effective and convenient means for guiding clinical application of medication.AimTo establish a method for determination of venlafaxine and its active metabolite O-desmethylvenlafaxine in human plasma by high-performance liquid chromatography with fluorescence detection.MethodsChromatographic separation was achieved on an Agilent Eclipse XDB-C18 Column (4.6 × 150 mm, 5 µm) with water containing sodium dihydrogen phosphate (0.05 mol/L) and acetonitrile (72:28) as the mobile phases. The following parameters were employed: flow rate 0.5 mL/min, column temperature 30°C, fluorescence excitation wavelength 276 nm and emission wavelength 598 nm.ResultsThe method showed good linearity in the concentration range 10–1000 ng/mL. The regression equation for venlafaxine was R=0.0054C+0.0264, r2=0.99991. The regression equation for O-desmethylvenlafaxine was R=0.0034C+0.0272, r2=0.99969. The intraday and interday precisions (relative SD) were less than 10%, and the quantitative limit was 10 ng/mL.ConclusionWe established a sensitive, specific and simple method for the detection of venlafaxine and O-desmethylvenlafaxine. This method fully meets the needs of clinical trials of venlafaxine and the requirements of relevant guidelines. It provided a reference for the clinical detection of venlafaxine and O-desmethylvenlafaxine plasma concentrations and pharmacokinetic study.

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

Molecules ◽  
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.

scholarly journals A Simple Determination of Mizoribine in Human Plasma by Liquid Chromatography with UV Detection

2005 ◽  
Vol 88 (4) ◽  
pp. 1114-1117 ◽  
Author(s):  
Hiroaki Kaji ◽  
Takayoshi Maiguma ◽  
Yoko Inukai ◽  
Hiroshige Ono ◽  
Ritsuko Taniguchi ◽  
...  
Keyword(s):  
Renal Function ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Plasma Concentrations ◽  
Peak Height ◽  
Therapeutic Drug ◽  
Simple Liquid ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A simple liquid chromatography (LC) method was developed for determination of the therapeutic level of mizoribine in human plasma. After precipitation of plasma proteins with 6% perchloric acid, mizoribine was determined by LC with spectophotometric detection. The peak height for mizoribine was linearly related to its concentrations, which ranged from 0.09 to 3.13 μg/mL. Therefore, the limit of quantitation was considered to be 0.09 μg/mL. The accuracy was 104.96–107.37%. The intra- and interday relative standard deviation values were in the range of 1.10–3.25%. The detection limit was 0.025 μ g/mL, defined as a signal-to-noise ratio of 3. The plasma concentrations of mioribine were not related to the dosage. Because mizoribine was mainly excreted in the urine, the plasma concentrations of mizoribine might be affected by a change in renal function. Therefore, the mizoribine concentration in blood should be monitored and the dosage adjusted, depending on the condition of renal function. It was suggested that the present method may be applied well in the therapeutic drug monitoring for mizoribine.

An HPLC method for simultaneous quantification of sunitinib and its active metabolite, SU12662, using hydrophilic interaction chromatography principle

Bioanalysis ◽  
2020 ◽  
Vol 12 (2) ◽  
pp. 75-85 ◽  
Author(s):  
Murari Gurjar ◽  
Parsshava Mehta ◽  
Jyoti Sharma ◽  
Sneha Patil ◽  
Preeti Kulkarni ◽  
...  
Keyword(s):  
Human Plasma ◽  
Active Metabolite ◽  
Internal Standard ◽  
Hplc Method ◽  
Therapeutic Drug ◽  
Hydrophilic Interaction ◽  
Reliable Determination ◽  
The Us ◽  
Us Fda

Aim: To develop a sensitive HPLC method for the quantitation of sunitinib (SU) and its active metabolite N-desethyl-sunitinib (SU12662) in human plasma. Materials & methods: The analytes were extracted from 500 μl of plasma using liquid–liquid extraction followed by protein precipitation. Chromatographic separation of two analytes and internal standard, vandetenib, was achieved on a hydrophilic interaction liquid chromatography analytical column using a gradient program. Calibration curves were linear over the range of 10–250 ng/ml for both SU and SU12662. The method was validated according to the US FDA guidelines for bioanalytical methods. Accuracy of the method at 10 ng/ml for SU and SU12662 was 8.7 and 6.7%, respectively, and precision was 10.18% and 17.3%, respectively. Conclusion: This method allows a specific, sensitive and reliable determination of SU and SU12662 in human plasma in a single analytical run which makes it useful for therapeutic drug monitoring.

scholarly journals Validation of a Capillary Electrophoresis Method for the Simultaneous Determination of Amlodipine Besylate and Valsartan in Pharmaceuticals and Human Plasma

2011 ◽  
Vol 94 (2) ◽  
pp. 498-502 ◽  
Author(s):  
Ahmed O Alnajjar
Keyword(s):  
Capillary Electrophoresis ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
Array Detector ◽  
Therapeutic Drug ◽  
Column Temperature ◽  
Photodiode Array Detector ◽  
Electrophoresis Method ◽  
Photodiode Array

Abstract A rapid, simple, and sensitive capillary electrophoresis (CE) method was developed and validated for the simultaneous determination of amlodipine (AML) and valsartan (VAL) in pharmaceuticals and human plasma using a UV photodiode array detector. Electrophoretic conditions were optimized to improve separation, sensitivity, and rapidity. The optimal conditions were 25 mM phosphate buffer at pH 8.0, injection time 10.0 s, voltage 25 kV, and column temperature 25C, with detection at 214 nm. The method was found to be linear in the range of 1.035 and 1.0350 mg/L, with weighted regression 0.9999 and 0.9994, for AML and VAL, respectively. Validation of the method showed acceptable intraday and interday accuracy (85.595.3) and precision (RSD 1.644.2) in pharmaceutical formulation and human plasma analysis. The sensitivity of the method was enhanced by both optimization of the CE procedure and preconcentration performed by liquidliquid extraction. The LOD for both AML and VAL was 0.03 mg/L, which allows analysis at the level of the drugs possibly found in human plasma. Therefore, the proposed method is suitable for QC in pharmaceutical laboratories and therapeutic drug monitoring in clinical laboratories.

scholarly journals Simultaneous Determination of Eight β-Lactam Antibiotics, Amoxicillin, Cefazolin, Cefepime, Cefotaxime, Ceftazidime, Cloxacillin, Oxacillin, and Piperacillin, in Human Plasma by Using Ultra-High-Performance Liquid Chromatography with Ultraviolet Detection

2016 ◽  
Vol 60 (8) ◽  
pp. 4734-4742 ◽  
Author(s):  
Tiphaine Legrand ◽  
Dominique Vodovar ◽  
Nicolas Tournier ◽  
Nihel Khoudour ◽  
Anne Hulin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Internal Standard ◽  
Therapeutic Drug ◽  
Simple Method ◽  
Validation Parameters

ABSTRACTA simple and rapid ultra-high-performance liquid chromatography (UHPLC) method using UV detection was developed for the simultaneous determination of eight β-lactam antibiotics in human plasma, including four penicillins, amoxicillin (AMX), cloxacillin (CLX), oxacillin (OXA), and piperacillin (PIP), and four cephalosporins, cefazolin (CFZ), cefepime (FEP), cefotaxime (CTX), and ceftazidime (CAZ). One hundred-microliter samples were spiked with thiopental as an internal standard, and proteins were precipitated by acetonitrile containing 0.1% formic acid. Separation was achieved on a pentafluorophenyl (PFP) column with a mobile phase composed of phosphoric acid (10 mM) and acetonitrile in gradient elution mode at a flow rate of 500 μl/min. Detection was performed at 230 nm for AMX, CLX, OXA, and PIP and 260 nm for CFZ, FEP, CTX, and CAZ. The total analysis time did not exceed 13 min. The method was found to be linear at concentrations ranging from 2 to 100 mg/liter for each compound, and all validation parameters fulfilled international requirements. Between- and within-run accuracy errors ranged from −5.2% to 11.4%, and precision was lower than 14.2%. This simple method requires small-volume samples and can easily be implemented in most clinical laboratories to promote the therapeutic drug monitoring of β-lactam antibiotics. The simultaneous determination of several antibiotics considerably reduces the time to results for clinicians, which may improve treatment efficiency, especially in critically ill patients.

scholarly journals Determination of Clobazam and Its Major Metabolite N-desmethylclobazam in Human Plasma with High-Performance Liquid Chromatography

Analytica ◽  
2021 ◽  
Vol 2 (3) ◽  
pp. 57-65
Author(s):  
Fadumo Ahmed Isse ◽  
Sherif Hanafy Mahmoud
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Practical Method ◽  
Therapeutic Drug ◽  
Reverse Phase ◽  
Simple Method ◽  
Metabolite Concentrations

Clobazam (CLB) is a benzodiazepine that is used in many types of epilepsy. Although therapeutic drug monitoring (TDM) of CLB is not routine, there is evidence that TDM may be of value in conditions where pharmacokinetic alterations are suspected. Therefore, determination of both CLB and its active metabolite concentrations is essential for TDM. Herein, we present a simple and practical method for determination of CLB and N-desmethylclobazam (NDMCLB) in human plasma by high-performance liquid chromatography (HPLC). The drugs were extracted by hexane:dichloromethane (1:1, v/v) from 0.3 mL plasma. The separation was carried out with a C18 reverse phase column using a mobile phase of water:acetonitrile (57:43, v/v) pumped at 0.8 mL/min. The analytes were detected at 228 nm. The method was linear over the concentration range 20–500 ng/mL for CLB and 200–3000 ng/mL for NDMCLB. The intra-day coefficient of variation (CV) was <10% for CLB and <6% for NDMCLB, while the inter-day CV for CLB was <16%. The metabolite inter-day CV was <6%. The accuracy of intra- and inter-day assessments determined for CLB and NDMCLB was within ±10%. This paper describes a rapid, reliable, and simple method for measuring CLB and its metabolite NDMCLB in human plasma. This UV-HPLC procedure offers acceptable precision and accuracy to quantify CLB and its metabolite in human plasma.

A Validated 2D-LC-UV Method for Simultaneous Determination of Imatinib and N-demethylimatinib in Plasma and Its Clinical Application for Therapeutic Drug Monitoring with GIST Patients

2020 ◽  
Vol 17 ◽  
Author(s):  
Houli Li ◽  
Di Zhang ◽  
Xiaoliang Cheng ◽  
Qiaowei Zheng ◽  
Kai Cheng ◽  
...  
Keyword(s):  
Therapeutic Drug Monitoring ◽  
One Dimension ◽  
Therapeutic Drug ◽  
Plasma Samples ◽  
Column Temperature ◽  
Injection Volume ◽  
Target Analytes ◽  
The One ◽  
Middle Column

Background: The trough concentration (Cmin) of Imatinib (IM) is closely related to the treatment outcomes and adverse reactions of patients with gastrointestinal stromal tumors (GIST). However, the drug plasma level has great interand intra-individual variability, and therapeutic drug monitoring (TDM) is highly recommended. Objective: To develop a novel, simple, and economical two-dimensional liquid chromatography method with ultraviolet detector (2D-LC-UV) for simultaneous determination of IM and its major active metabolite, N-demethyl imatinib (NDIM) in human plasma, and then apply the method for TDM of the drug. Method: Sample was processed by simple protein precipitation. Two target analytes were separated on the one-dimension column, captured on the middle column, and then transferred to the two-dimension column for further analysis. The detection was performed at 264 nm. The column temperature was maintained at 40˚C and the injection volume was 500 μL. Totally 32 plasma samples were obtained from patients with GIST who were receiving IM. Method: Sample was processed by simple protein precipitation. Two target analytes were separated on the one-dimension column, captured on the middle column, and then transferred to the two-dimension column for further analysis. The detection was performed at 264 nm. The column temperature was maintained at 40˚C and the injection volume was 500 μL. Totally 32 plasma samples were obtained from patients with GIST who were receiving IM. Conclusion: The novel 2D-LC-UV method is simple, stable, highly automated and independent of specialized technicians, which greatly increases the real-time capability of routine TDM for IM in hospital.

RADIOIMMUNOASSAY FOR 2-METHOXYOESTRONE IN HUMAN PLASMA

1979 ◽  
Vol 91 (1) ◽  
pp. 158-166 ◽  
Author(s):  
Günter Emons ◽  
Peter Ball ◽  
Gertrud v. Postel ◽  
Rudolf Knuppen
Keyword(s):  
Human Plasma ◽  
Plasma Concentrations ◽  
Cross Reactivity ◽  
Elderly Men ◽  
Specific Antibodies ◽  
Assay Procedure ◽  
Menopausal Women ◽  
Bovine Serum Albumin Conjugate ◽  
Post Menopausal

ABSTRACT A bovine serum albumin conjugate of 2-methoxyoestrone was used for the preparation of highly specific antibodies in rabbits. Cross-reactivity for catecholoestrogens and monophenolic steroids was below 0.3 %. Only 2-methoxyoestradiol cross-reacted with 44 %. An assay procedure for the determination of unconjugated and conjugated 2-methoxyoestrone in human plasma is described. The following mean plasma concentrations (pg/ml) were found (unconjugated/conjugated): children 61/1130, young men 74/1320, elderly men 109/1260, cycling women 131/1040, post-menopausal women 102/1420, and pregnant women 3980/5850.

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

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
Sign in / Sign up

Export Citation Format

Share Document