scholarly journals ESTIMATION OF ETONOGESTREL IN HUMAN PLASMA BY USING LC–ESI–MS/MS METHOD

2017 ◽  
Vol 9 (12) ◽  
pp. 147
Author(s):  
Satish Ramanatham Velamakanni ◽  
Venkateswarlu Padala
Keyword(s):  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Chromatographic Method ◽  
Internal Standard ◽  
Assay Method ◽  
Pharmacokinetic Studies ◽  
Linear Calibration ◽  
Sensitivity Matrix ◽  
Liquid Liquid Extraction ◽  
Healthy Females

Objective: The aspiration of the present study was to develop simple, robust and reliable liquid chromatography/electro spray ionization tandem mass spectrometry (LC-MS/MS) (Agilent Technologies) assay method for the quantification of etonogestrel in human serum by using etonogestrel d6 as internal standard (IS).Methods: An easy Liquid-Liquid Extraction (LLE) sample processing method was used to extract etonogestrel from plasma and chromatographic method was developed with run time 3.5min with linear calibration curve ranges from 50-3604 pg/mL for both etonogestrel and etonogestrel d6 and chromatographic method validated by determining carryover test, sensitivity, matrix effect, linearity, precision, accuracy, recovery, dilution integrity and stability. The developed method was used for pharmacokinetic study of 75mcg desogestrel tablet formulation under fasting condition in healthy females.Results: The validation showed the developed method was accurate with the results of validated parameters were met acceptance criteria as per Food and Drug Administration (FDA) guidelines. The validated method successfully was used for pharmacokinetic study of 75mcg desogestrel tablet in healthy females and quantified the amount of etonogestrel and IS.Conclusion: The developed method for etonogestrel in human plasma has been validated and used in pharmacokinetic studies. 

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 Investigation of Pharmacokinetic Parameters of Trelagliptin in Egyptian Volunteers Using Sensitive LC-MS/MS: A Comparative Study with a Japanese Population

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Shereen Mowaka ◽  
Nermeen Ashoush ◽  
Mariam M. Tadros ◽  
Bassam M. Ayoub
Keyword(s):  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Biological Fluids ◽  
Internal Standard ◽  
Pharmacokinetic Parameters ◽  
Antidiabetic Drug ◽  
Liquid Liquid Extraction ◽  
Direct Precipitation ◽  
Structure Similarity

Trelagliptin (TLN) is a novel once-weekly antidiabetic drug that enhanced the patient compliance in type 2 diabetes. TLN analysis and bioanalysis literature review showed many methods for TLN assay either in dosage form or as biological fluids (pharmacokinetic parameters), but all those methods did not consider the full details dealing with biological assay of TLN. Studies that included information about pharmacokinetic parameters did not mention the used analytical procedures for those determinations and parameters. Although some LC-MS/MS and UPLC-UV methods were reported for TLN bioassay in rats’ plasma, they used direct precipitation techniques, and the current described procedure showed lower LLOQ than all the reported methods in spite of that working on human plasma is more complicated than on rats’ plasma. In this study, LC-MS/MS bioanalysis of TLN in human plasma (4–1000 nM) was employed successfully with LLOQ of 4 nM which is lower than all reported methods in rats’ plasma followed by a preliminary pharmacokinetic study. Alogliptin was used as internal standard (IS) because of its structure similarity to TLN. Pharmacokinetic parameters of TLN were investigated in Egyptian volunteers, and they had been compared to Japanese. Liquid-liquid extraction showed more sensitive results than direct precipitation. The proposed method was successfully applied to a pharmacokinetic study conducted on Egyptian volunteers. No dose modification is required upon comparing the pharmacokinetic parameters of the current study and previous studies on non-Egyptian volunteers.

Determination of Acotiamide in human plasma by LC-MS/MS and its application to a pharmacokinetic study

2020 ◽  
Vol 17 ◽  
Author(s):  
Qian Sun ◽  
Qiao-gen Zou ◽  
Yun-yan Xia ◽  
Cheng-qun Han
Keyword(s):  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Ammonium Acetate ◽  
Internal Standard ◽  
Rat Plasma ◽  
Pharmacokinetic Studies ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Tandem Mass Spectrometric

Background: A liquid chromatography-tandem mass spectrometric (LC-MS/MS) method had been developed for the quantification of acotiamide in rat plasma and been applied to pharmacokinetic studies. However, there was no LC-MS/MS method been developed for the determination of acotiamide in human plasma and its pharmacokinetic study. Objective: A simple and fast LC-MS/MS method was established and validated for the quantification of acotiamide in human Received: plasma and was applied to a pharmacokinetic study. Methods: Sample preparation was accomplished Revised: Accepted: through protein precipitation, and chromatographic separation was achieved on a Welch, Ultimate XB-C18 column (2.1×50 mm, 3 μm) with a security guard cartridge C18 using a binary gradient with DOI: mobile phase A (Methanol) and B (the solution of 10 mM Ammonium acetate with 0.1% Formic acid) at a flow rate of 400 Results: The retention time of acotiamide and its internal standard, acotiamide-d6 was 1.78 min and 1.79 min, respectively. The total run time was 4.0 min. The method was developed and validated over the concentration range of 0.500-100 ng/mL for acotiamide, with correlation coefficient greater than 0.9987. The extraction recovery was more than 108.43% and the matrix effect was not significant. The inter- and intra-day precisions were below 5.80% and accuracies ranged from 92.7 to 103.0%. Acotiamide was demonstrated to be stable in human plasma under the tested conditions. Conclusion: The validated LC-MS/MS method was successfully applied to study the pharmacokinetic profiles of acotiamide in human plasma after oral administration and has achieved satisfactory results.

scholarly journals Improved HPLC Method for the Determination of Moxifloxacin in Application to a Pharmacokinetics Study in Patients with Infectious Diseases

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Nan Wang ◽  
Liqin Zhu ◽  
Xuequn Zhao ◽  
Wenjie Yang ◽  
He Sun
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Hplc Method ◽  
Single Step ◽  
Pharmacokinetic Studies ◽  
Liquid Liquid Extraction ◽  
High Concentrations

Objective. To develop a simple and rapid high-performance liquid chromatography (HPLC) method for measuring moxifloxacin concentration in human plasma. Methods. Following a single step liquid-liquid extraction, analytes along with an internal standard (IS) were separated using an isocratic mobile phase of 0.1% triethylamine (adjusted pH to 4.8 with phosphoric acid)/acetonitrile (80/20, v/v) at flow rate of 1 mL/min on reverse phase Kromasil C18 column (250 mm × 4.6 mm, 5 μm) at room temperature. Results. Total analytical run time for selecting moxifloxacin was 15 min. The assays exhibited good linearity (r2=0.9998) over the studied range of 25 to 5000 ng/mL. The absolute recovery rate of low, medium, and high concentrations were 69.88%, 78.86%, and 78.51%, respectively. The relative recovery rates were 98.50%, 96.61%, and 101.79%, respectively. Coefficient of variation and error at both of the intraday and interday assessments were less than 4.7%. Conclusions. The results indicated that this method is a simple, rapid, precise and accurate assay for the determination of moxifloxacin concentrations in human plasma. This validated method is sensitive and reproducible enough to be used in pharmacokinetic studies.

scholarly journals Improved HPLC Method for Determination of Four PPIs, Omeprazole, Pantoprazole, Lansoprazole and Rabeprazole in Human Plasma

2010 ◽  
Vol 13 (1) ◽  
pp. 1 ◽  
Author(s):  
Maryam Noubarani ◽  
Fariborz Keyhanfar ◽  
Manijeh Motevalian ◽  
Masoud Mahmoudian
Keyword(s):  
Human Plasma ◽  
Room Temperature ◽  
Internal Standard ◽  
Cost Benefit ◽  
Hplc Method ◽  
Single Step ◽  
Pharmacokinetic Studies ◽  
Limit Of Quantification ◽  
Liquid Liquid Extraction

ABSTRACT-PURPOSE: To develop a simple and rapid HPLC method for measuring of four proton-pump inhibitors (PPIs), omeprazole (OPZ), pantoprazole (PPZ), lansoprazole (LPZ) and rabeprazole (RPZ) concentrations in human plasma. METHODS: Following a single step liquid–liquid extraction analytes along with an internal standard (IS) were separated using an isocratic mobile phase of phosphate buffer (10 mM)/acetonitrile (53/47, v/v adjusted pH to 7.3 with triethylamine) at flow rate of 1 mL/min on reverse phase TRACER EXCEL 120 ODS-A column at room temperature. RESULTS: Total analytical run time for selected PPIs was 10 min. The assays exhibited good linearity (r2>0.99) over the studied range of 20 to 2500 ng/mL for OPZ, 20 to 4000 ng/mL for PPZ, 20 to 3000 ng/mL for LPZ and 20 to 1500 ng/mL for RPZ. The recovery of method was equal or greater than 80% and lower limit of quantification (LLOQ) was 20 ng/mL for four PPIs. Coefficient of variation and error at all of the intra-day and inter-day assessment were less than 9.2% for all compounds. CONCLUSIONS: The results indicated that this method is a simple, rapid, precise and accurate assay for determination of four PPIs concentrations in human plasma. This validated method is sensitive and reproducible enough to be used in pharmacokinetic studies and also is time- and cost-benefit when selected PPIs are desired to be analyzed.

scholarly journals Development and Validation of Novel HPLC Bioanalytical Analysis Method for Acalabrutinib: An Anticancer Drug in Human Plasma

2020 ◽  
Vol 32 (10) ◽  
pp. 2606-2610
Author(s):  
G. Atchutarama Krishna ◽  
P. Srinivasarao ◽  
T. Benarji Patrudu ◽  
R. Chidanandaswamy
Keyword(s):  
Human Plasma ◽  
Orthophosphoric Acid ◽  
Internal Standard ◽  
Hplc Method ◽  
Linear Calibration ◽  
Liquid Liquid Extraction ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Development And Validation

The aim of the work is to develop and validate the bioanalytical RP-HPLC method for determination of acalabrutinib in plasma with nifedipine drug as internal standard. Liquid-liquid extraction with diethyl ether and methanol in the ratio of 50:50 (v/v) was used for the extraction of drugs from the biological matrix. The optimized chromatography conditions consist of methanol, acetonitrile and 0.1% orthophosphoric acid in the ratio of 45:35:20 (v/v) as a mobile phase with KNAUER Eurospher II C18 Column (250 × 4.6 mm, 5μ) as stationary phase. Isocratic elution with 0.9 mL flow separates acalabrutinib at 4.6 min and nifedipine at 6.8 min. The method was validated as per ICH guidelines and linear calibration curve was obtained for the peak area ratio of acalabrutinib and nifedipine compound across a range of 50-3000 ng/mL. Greater than 90% recoveries were obtained for acalabrutinib. The relative standard deviation (%RSD) was found to be < 5% for precision studies. Hence, the method was found to be suitable for the analysis of acalabrutinib in spiked human plasma and is used for the pharmacokinetic study

Development and Validation of a New Method for the Determination of Anti-hepatitis C Agent Simeprevir in Human Plasma using HPLC with Fluorescence Detection

2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil
Keyword(s):  
Hepatitis C ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Assay Method ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Relative Standard

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.

Bioanalytical method development and validation of simultaneous analysis of telmisartan and hydrochlorthiazide in human plasma using LC-MS/MS

2016 ◽  
Vol 5 (03) ◽  
pp. 4862 ◽  
Author(s):  
Mathew George* ◽  
Lincy Joseph ◽  
Arpit Kumar Jain ◽  
Anju V.
Keyword(s):  
Human Plasma ◽  
Retention Time ◽  
High Performance ◽  
Method Development ◽  
Matrix Effects ◽  
Solid Phase ◽  
Internal Standard ◽  
Assay Method ◽  
Buffer System ◽  
Internal Standards

A simple, sensitive, rapid and economic high performance thin layer chromatographic method and a mass spectroscopic assay method has been developed for the quantification of telmisartan and hydrochlorthiazide combination in human plasma. The internal standards and analytes were extracted from human plasma by solid-phase extraction with HLB Oasis1cc (30mg) catridges. The scanning and optimization for the samples are done using methanol: water (50:50). The samples were chromatographed using reverse phase chromatography with C-18 column of different manufacturers like Ascentis C18 (150×4. 6, 5µ) using the buffer system Acetonitrile: Buffer (80:20%v/v) which consist of 2±0. 1Mm ammonium format at a flow rate of 0. 7ml/min at a column oven temperature 35±10c. The internal standard used was hydrochlorthiazide13c1, d2 and telmisartand3. The extraction techniques include conditioning, loading, washing and elution, drying followed by reconstitution of the dried samples. The volume injected was 10µl with the retention time of 3-4 min for telmisartan, 1-2 min for hydrochlorthiazide and for the internal standards the retention time was 3-4 min for telmisartand3 and 1-2 min for hydrochlorthiazide c13d2. The rinsing solution was Acetonitrile: HPLC grade water in the ratio (50:50). The above developed method was validated using various parameters like selectivity and sensitivity, accuracy and precision, matrix effects, % recovery and various stability studies. The method was proved to be sensitive, accurate, precise and reproducible. The preparation showed high recovery for the quantitative determination of telmisartan and hydrochlorthiazide in human plasma.

scholarly journals Determination of sarecycline by UPLC-MS/MS and its application to pharmacokinetic study in rats

2020 ◽  
Author(s):  
Yonghui Shen ◽  
Deru Meng ◽  
Feifei Chen ◽  
Hui Jiang ◽  
Liming Hu ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Chronic Inflammatory Disease ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Acquity Uplc ◽  
Intravenous And Oral Administration

AbstractSarecycline is a narrow-spectrum antibiotic for the treatment of acne, which is a chronic inflammatory disease of the hair follicle sebaceous glands. In the study, UPLC-MS/MS was used to establish a rapid and accurate analytical method. The sarecycline was determined with poziotinib as internal standard (IS) in rat plasma. An ACQUITY UPLC HSS T3 column (2.1 × 100 mm, 1.8 μm) could performe chromatographic separation with the mobile phase (methanol: water of 0.1% formic acid) with gradient elution. The ions of target fragment were m/z 488.19→410.14 for sarecycline and m/z 492.06→354.55 for poziotinib, which could quantify the electrospray ionization of positive multiple reaction monitoring (MRM) mode. The linear calibration curve of the concentration range was 1–1,000 ng/mL for sarecycline with a lower limit of quantification (LLOQ) of 1 ng/mL. The mean recovery was between 82.46 and 95.85% for sarecycline and poziotinib in rat plasma. RSD for precision of inter-day and intra-day were between 3.24 and 13.36%, and the accuracy ranged from 105.26 to 109.75%. The developed and validated method was perfectly used in the pharmacokinetic study and bioavailability of sarecycline after intravenous and oral administration in rats.

Sign in / Sign up

Export Citation Format

Share Document