Application of LC–MS/MS method for determination of dihydroartemisin in human plasma in a pharmacokinetic study

Bioanalysis ◽  
2020 ◽  
Vol 12 (22) ◽  
pp. 1635-1646
Author(s):  
Huanhuan Wang ◽  
Xueting Yao ◽  
Teng Wang ◽  
Shuai Yan ◽  
Ji Jiang ◽  
...  
Keyword(s):  
Human Plasma ◽  
Lupus Erythematosus ◽  
Bioanalytical Methods ◽  
Therapeutic Potential ◽  
Pharmacokinetic Profile ◽  
Internal Standards ◽  
Ionization Mode ◽  
Spe Method ◽  
Reliable Analytical Method

Aim: Dihydroartemisinin (DHA) was also found therapeutic potential for the treatment of systemic lupus erythematosus (SLE). To assess the pharmacokinetic profile of DHA, the concentration of DHA in plasma of SLE patients needed be accurately determined based on a rapid and reliable analytical method. Experimental method & results: Developed method utilizes stable isotope-labeled internal standards and SPE method for sample preparation, applied XBridge C18 column (2.1 × 50 mm, 3.5 μm) for chromatography separation. Detection of the analytes was achieved by an AB Sciex 4000 mass spectrometer under positive electrospray ionization mode. The method was validated in accordance with international guidelines on bioanalytical methods validations. Conclusion: DHA concentrations in human plasma of Chinese SLE patients were quantified by developed LC–MS/MS (no. 2016L02562).

A sensitive liquid-chromatographic method for determination of 3'-azido-3'-deoxythymidine (AZT) in plasma and urine.

1988 ◽  
Vol 34 (8) ◽  
pp. 1565-1568 ◽  
Author(s):  
M A Hedaya ◽  
R J Sawchuk
Keyword(s):  
Human Plasma ◽  
Prescription Drugs ◽  
Chromatographic Method ◽  
Internal Standard ◽  
Infectious Complications ◽  
Over The Counter ◽  
Internal Standards ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic assay for AZT in human plasma and urine. This assay involves the use of two internal standards, allowing reference of AZT peaks to the appropriate internal standard, the choice depending on the range of concentrations encountered. This method is isocratic, specific, sensitive enough to allow quantification of AZT in concentrations observed clinically, and requires only 13 min of chromatographic time. We saw no interference from various over-the-counter and prescription drugs often used in treating the infectious complications of AIDS.

UHPLC–MS/MS method to determine FP-208 in human plasma and its application to a pharmacokinetic study

Bioanalysis ◽  
2020 ◽  
Vol 12 (6) ◽  
pp. 367-378
Author(s):  
Huanhuan Wang ◽  
Teng Wang ◽  
Zhanqing Wang ◽  
Zhenjian Du ◽  
Qian Zhao ◽  
...  
Keyword(s):  
Solid Tumors ◽  
Mammalian Target Of Rapamycin ◽  
Human Study ◽  
Pharmacokinetic Profile ◽  
Target Of Rapamycin ◽  
Precipitation Method ◽  
Molecule Inhibitor ◽  
Ionization Mode ◽  
First Time ◽  
Reliable Analytical Method

Aim: FP-208 is a novel and effective small-molecule inhibitor blocking the mammalian target of rapamycin complex-1/mammalian target of rapamycin complex-2/PI3Ka. To investigate the pharmacokinetic profile of FP-208, a rapid and reliable analytical method was needed to be established to determine FP-208 in the plasma of patients with solid tumors. Materials & methods: FP208 was separated on a charged surface hybrid (CSH) C18 column (2.1 mm × 50 mm, 1.7 μm) after the plasma samples were purified using a protein precipitation method. Detection was performed on an AB Sciex 5500 mass spectrometer in the positive electrospray ionization mode. The established method was validated according to the bioanalytical guidelines. Conclusion: For the first time, the developed and validated method was successfully applied in the first-in-human study for FP-208 in patients with solid tumors after oral administration (Number: CTR20180683).

scholarly journals Determination of nimodipine in plasma by HPLC-MS/MS and pharmacokinetic application

2010 ◽  
Vol 46 (4) ◽  
pp. 665-677 ◽  
Author(s):  
Demétrius Fernandes do Nascimento ◽  
Manoel Odorico de Moraes ◽  
Fernando Antônio Frota Bezerra ◽  
Andréa Vieira Pontes ◽  
Célia Regina Amaral Uchoa ◽  
...  
Keyword(s):  
Human Plasma ◽  
Internal Standard ◽  
Pharmacokinetic Profile ◽  
Plasma Samples ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Standard Curve ◽  
Liquid Liquid Extraction ◽  
Highly Sensitive

To develop and validate a rapid, specific and highly sensitive method to quantify nimodipine in human plasma using dibucaine as the internal standard (IS). The analyte and IS were extracted from plasma samples by liquid-liquid extraction using hexane-ethyl acetate (1:1 v/v). The chromatographic separation was performed on a Varian® Polaris C18 analytical column (3 μm, 50 x 2.0 mm) and pre-column SecurityguardTM C18 (4.0 x 3.0 mm) with a mobile phase of Acetonitrile-Ammonium acetate 0.02 ml/L (80:20v/v). The method had a chromatographic run time of 4.5 min and linear calibration curve over the range of 0.1- 40 ng/mL (r > 0.9938). The limit of quantification was 100 pg/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges. This validated method was successfully applied in determining the pharmacokinetic profile of nimodipine tablets of 30 mg administered to 24 healthy volunteers. The proposed method of analysis provided a sensitive and specific assay for nimodipine determination in human plasma. The time for the determination of one plasma sample was 4.5 min. This method is suitable for the analysis of nimodipine in human plasma samples collected for pharmacokinetic, bioavailability or bioequivalence studies in humans.

scholarly journals Simultaneous LC-MS/MS Determination of Sacubitril, Valsartan and LBQ657 in Human Plasma and Its Application to Clinical Study

2021 ◽  
Author(s):  
Yufeng Ni ◽  
Yujia Zhang ◽  
Chong Zou ◽  
Li Ding
Keyword(s):  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Ionization Source ◽  
Internal Standards ◽  
Accuracy And Precision ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Positive Ion

A rapid and reproducible liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine sacubitril, valsartan and a metabolite of sacubitril (LBQ657) in human plasma using sacubitril-d4 and valsartan-d3 as the internal standards. Following protein precipitation, the analytes were operated on an Ultimate® XB-C18 column (2.1 × 50 mm, 3.5 μm, Welch) with a gradient elution with acetonitrile, and 5 mM ammonium acetate and 0.1% formic acid in water as the mobile phase. The detection was performed on a Triple Quad™ 4000 mass spectrometer coupled with an electrospray ionization source (ESI) under positive-ion multiple reaction monitoring mode. The linearities are 2.00-4000, 5.00-10000 and 5.00-10000 ng mL-1 for sacubitril, valsartan and LBQ657, respectively. The accuracy and precision of intra- and inter-day, dilution accuracy, recovery and stability of the method were all within the acceptable limits and no matrix effect or carryover was observed. The suitability of the method was successfully demonstrated in terms of the quantification of sacubitril, valsartan and LBQ657 in plasma samples collected from healthy Chinese volunteers in a clinical trial.

Determination of doravirine in human plasma using liquid–liquid extraction and HPLC–MS/MS

Bioanalysis ◽  
2019 ◽  
Vol 11 (16) ◽  
pp. 1495-1508
Author(s):  
Rajesh Desai ◽  
Brad Roadcap ◽  
Dina Goykhman ◽  
Eric Woolf
Keyword(s):  
Human Plasma ◽  
Dynamic Range ◽  
Multiple Reaction Monitoring ◽  
Development Program ◽  
Liquid Extraction ◽  
Clinical Development Program ◽  
Liquid Liquid Extraction ◽  
Multiple Reaction Monitoring Mode ◽  
Ionization Mode

Aim: A method to quantitate doravirine (MK-1439) in human plasma has been developed to support human clinical trials designed to evaluate the safety, pharmacokinetics and efficacy of the compound. Methodology & results: The analyte was extracted using liquid–liquid extraction, separated on a reverse phase HPLC column, and detected on an API-4000 mass spectrometer using a Turbo-Ion spray source in positive ionization mode coupled with multiple reaction monitoring mode was used for quantification. The dynamic range for the assay was 0.02–10 ng/ml using 100 μl of human plasma. Conclusion: The assay was found to be sensitive, selective and reproducible and applied to support the doravirine clinical development program.

Simultaneous Bioanalysis of Prodrug Oseltamivir and its Metabolite Oseltamivir Carboxylic Acid in Human Plasma by LC/MS/MS Method and its Application to Disposition Kinetics

2020 ◽  
Vol 16 (2) ◽  
pp. 143-152
Author(s):  
Dodda Sireesha ◽  
Makula Ajitha ◽  
Kandhagatta Raj Narayana
Keyword(s):  
Carboxylic Acid ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standards ◽  
South Indian ◽  
Liquid Chromatography Tandem Mass ◽  
Incurred Sample Reanalysis ◽  
Oseltamivir Phosphate ◽  
Male Subjects

Introduction: A selective, sensitive, precise and rapid analytical method using liquid chromatography- tandem mass spectrometry (LC/MS/MS) for simultaneous determination of oseltamivir and oseltamivir carboxylic acid in plasma has been developed and validated, using oseltamivir-D5 and oseltamivir acid-D3 as internal standards. Methods: The analytes were extracted from 300μL of human plasma using solid phase extraction technique. A mixture of methanol and 0.1% formic acid (60:40, v/v) was used as mobile phase at a flow rate of 0.7mL/min, to separate the analytes on Zorbax SB-C18 (50x4.6mm, 3.5μm) analytical column. Results: The calibration curves obtained were linear over the concentration ranges of 0.5-200ng/mL and 2.0-800ng/mL for oseltamivir and oseltamivir carboxylic acid respectively. A run time of 2.5min makes it possible to analyze more than 350 plasma samples in a day, thereby increasing the productivity. Conclusion: The present method was applied successfully to a clinical pharmacokinetic study in South Indian male subjects with 75mg oseltamivir phosphate capsule under fasting conditions and the results were authenticated by incurred sample reanalysis.

A Sensitive LC–MS/MS Method for the Determination of Afatinib in Human Plasma and Its Application to a Bioequivalence Study

2021 ◽  
Author(s):  
Xi Luo ◽  
Xiu Jin Zhang ◽  
Wen Ling Zhu ◽  
Jin Ling Yi ◽  
Wen Gang Xiong ◽  
...  
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Ionization Mode

Abstract A high performance liquid chromatography–tandem mass spectrometry assay for the determination of afatinib (AFT) in human plasma was established. A simple sample preparation of protein precipitation was used and separation was achieved on a C18 column by the gradient mixture of mobile Phase A of water (containing 0.1% ammonia) and the mobile Phase B of acetonitrile and water (V:V = 95:5, containing 0.2% ammonia). The multiple reaction monitoring mode was used to monitor the precursor-to-production transitions of m/z 486.2 → m/z 371.4 for AFT and m/z 492.2 → m/z 371.3 for AFT-d6 (internal standard) at positive ionization mode. The calibration curve ranged from 0.100 to 25.0 ng·mL−1 and the correlation coefficient was greater than 0.99. The intra- and inter-batch precision was less than or equal to 10.0%. Accuracy determined at four concentrations was in the range of 92.3–103.3%. In summary, our method was sensitive, simple and reliable for the quantification of AFT and was successfully applied to a bioequivalence study.

Simultaneous Determination of Alogliptin and Pioglitazone in Human Plasma by a Novel LC-MS/MS Method

2020 ◽  
Vol 16 (5) ◽  
pp. 564-577
Author(s):  
Duddukuru Sri Sesha Sai Praveen ◽  
Syed Asha ◽  
Ravi Kumar Pigili
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Solid Phase ◽  
Protein Precipitation ◽  
Detection Methods ◽  
Therapeutic Drug ◽  
Internal Standards ◽  
One Step ◽  
Precision And Accuracy

Background: A combination of alogliptin and pioglitazone is well tolerated. It does not increase the risk of hypoglycemia. In order to study the bioavailability of aloglipitn in the presence of pioglitazone, it is essential to have a method that can simultaneously detect both in human plasma. A protein precipitation-based method was used to determine alogliptin and pioglitazone simultaneously in human plasma. Protein precipitation causes ion suppression or enhancement in detection methods when compared to other methods. Objective: To simultaneously quantify alogliptin and pioglitazone in human plasma by LC-MS/MS based method. Methods: LC-MS/MS method for the simultaneous determination of pioglitazone and alogliptin in human plasma using stable isotope labelled compounds internal standards. The simple and one step solid phase extraction (SPE) was employed to extract the analytes from plasma. The extracted samples were separated on a C18 column by using a 25:75 (v/v) mixture of acetonitrile and 5 mM ammonium formate as the mobile phase at a flow rate of 0.5 mL/min. Results: The calibration curves obtained were linear (r2= 0.99) over the concentration range of 12.0- 2438.0 ng/mL for pioglitazone and 1.0-202.0 ng/mL for alogliptin. The results of the intra- and interday precision and accuracy studies were found to be within the acceptable limits. The analytes were stable under different stability conditions. All the validation results were found to be within the acceptable limits. The total analytical run time was 3.0 min. There was no interference from plasma matrices. Conclusion: The developed method is precise and adequately sensitive for detection and quantification of analytes. Thus, the method can be useful for bioavailability and bioequivalence (BA/BE) studies and routine therapeutic drug monitoring with the desired precision and accuracy.

Simultaneous Determination of Rosuvastatin, Rosuvastatin-5 S-lactone, and N-desmethyl Rosuvastatin in Human Plasma by UPLC-MS/MS and Its Application to Clinical Study

Drug Research ◽  
2017 ◽  
Vol 68 (06) ◽  
pp. 328-334 ◽  
Author(s):  
Xue Bai ◽  
Xi-Pei Wang ◽  
Guo-Dong He ◽  
Bin Zhang ◽  
Min Huang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Clinical Study ◽  
Human Plasma ◽  
Ultra Performance Liquid Chromatography ◽  
Internal Standards ◽  
Liquid Chromatography Tandem Mass ◽  
Artery Disease ◽  
Acquity Uplc ◽  
Positive Ion

Abstract Objective A rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) assay was developed and validated for the simultaneous quantification of rosuvastatin (RST), rosuvastatin-5 S-lactone (RSTL), and N-desmethyl rosuvastatin (DM-RST) in human plasma. Methods Sample was prepared by liquid-liquid extraction with ethyl acetate from 100 μL acidulated buffered plasma. Then analytes were chromatographically separated using an Acquity UPLC HSS T3 column (3.0 mm×100 mm, 1.8 µm) by 0.1% formic acid and gradient acetonitrile at a flow rate of 0.30 mL/min. Three analytes and internal standards (carbamazepine) were eluted in 3.5 min. Mass spectrometry detection was performed through positive ion electrospray ionization (ESI). Results The calibration curves for three analytes were linear (R≥0.9987, n=3) within the concentration range of 0.1–50 ng/mL for RST and RSTL, and 0.2–100 ng/mL for DM-RST. Mean extraction recoveries were enhanced by means of acidulated plasma using ammonium acetate of pH 4.0, which ranged within 75.3–98.8% for three analytes. Intra- and inter precision and accuracy were 88.2–96.4%. Conclusions This present method was lower LLOQ, less time consuming (3.5 min), less plasma consuming (100 µL) and simpler sample preparation. And it was successfully applied to determine steady state concentrations of RST, RSTL and DM-RST in a clinical study of RST for patients with coronary artery disease (CAD).

A simple and reliable analytical method for simultaneous quantification of first line antitubercular drugs in human plasma by LCMS/MS

2020 ◽  
Vol 12 (31) ◽  
pp. 3909-3917
Author(s):  
Bijoy Kumar Panda ◽  
Medha Bargaje ◽  
Sathiyanarayanan L.
Keyword(s):  
Human Plasma ◽  
Analytical Method ◽  
Reliable Method ◽  
First Line ◽  
Antitubercular Drugs ◽  
Simultaneous Quantification ◽  
Reliable Analytical Method

The present study describes the optimization of a simple and reliable method for the determination of four first line antitubercular drugs in human plasma.

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