scholarly journals Determination and Quantification of Phenytoin in Human Plasma by Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometry

2008 ◽  
Vol 5 (1) ◽  
pp. 169-176 ◽  
Author(s):  
S. M. N. Roy ◽  
S. M. Yetal ◽  
V. V. Vaidya ◽  
S. S. Joshi
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Simple Procedure ◽  
Internal Standard ◽  
Reversed Phase ◽  
Therapeutic Monitoring ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

A rapid and simple high pressure liquid chromatography method with mass spectrometry detection was developed and validated for the determination of phenytoin in human plasma. Metaxalone was used as internal standard. The sample preparation involves a rapid and simple procedure based on liquid-liquid extraction. Analysis was performed in less than 3.0 minutes in isocratic mode on a reversed phase C18column (5μ; 50 × 4.6 mm) using a mobile phase composed of acetonitrile-buffer 2 mM ammonium acetate (80:20v/v), pH of buffer adjusted to 3.4 using formic acid, at 0.4 mL min-1 flow rate. The calibration curves were linear in the measured range between 101.2 ng mL-1and 5060.0 ng mL-1. The validated lowest limit of quantification was 101.2 ng mL-1for phenytoin. The mean relative recovery for drug and Internal standard was found to be 78.33% and 77.04%, respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma.

scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

scholarly journals A Simple High-Performance Liquid Chromatography Method for Simultaneous Determination of Three Triazole Antifungals in Human Plasma

2012 ◽  
Vol 57 (1) ◽  
pp. 484-489 ◽  
Author(s):  
Mei Zhang ◽  
Grant A. Moore ◽  
Murray L. Barclay ◽  
Evan J. Begg
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Internal Standard ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatography Method

ABSTRACTA rapid and simple high-performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of three triazole antifungals (voriconazole, posaconazole, and itraconazole and the metabolite of itraconazole, hydroxyitraconazole) in human plasma. Sample preparation involved a simple one-step protein precipitation with 1.0 M perchloric acid and methanol. After centrifugation, the supernatant was injected directly into the HPLC system. Voriconazole, posaconazole, itraconazole, its metabolite hydroxyitraconazole, and the internal standard naproxen were resolved on a C6-phenyl column using gradient elution of 0.01 M phosphate buffer, pH 3.5, and acetonitrile and detected with UV detection at 262 nm. Standard curves were linear over the concentration range of 0.05 to 10 mg/liter (r2> 0.99). Bias was <8.0% from 0.05 to 10 mg/liter, intra- and interday coefficients of variation (imprecision) were <10%, and the limit of quantification was 0.05 mg/liter.

scholarly journals Liquid chromatography–tandem mass spectrometry for the simultaneous quantitation of ceftriaxone, metronidazole and hydroxymetronidazole in plasma from seriously ill, severely malnourished children

2017 ◽  
Vol 2 ◽  
pp. 43 ◽  
Author(s):  
Martin Ongas ◽  
Joseph Standing ◽  
Bernhards Ogutu ◽  
Joseph Waichungo ◽  
James A. Berkley ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Severe Acute Malnutrition ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Reversed Phase ◽  
Cefuroxime Axetil ◽  
Acute Malnutrition ◽  
Ionization Mass ◽  
Chromatography Method

We have developed and validated a novel, sensitive, selective and reproducible reversed-phase high-performance liquid chromatography method coupled with electrospray ionization mass spectrometry (HPLC–ESI-MS/MS) for the simultaneous quantitation of ceftriaxone (CEF), metronidazole (MET) and hydroxymetronidazole (MET-OH) from only 50 µL of human plasma, and unbound CEF from 25 µL plasma ultra-filtrate to evaluate the effect of protein binding. Cefuroxime axetil (CEFU) was used as an internal standard (IS). The analytes were extracted by a protein precipitation procedure with acetonitrile and separated on a reversed-phase Polaris 5 C18-Analytical column using a mobile phase composed of acetonitrile containing 0.1% (v/v) formic acid and 10 mM aqueous ammonium formate pH 2.5, delivered at a flow-rate of 300 µL/min. Multiple reaction monitoring was performed in the positive ion mode using the transitions m/z555.1→m/z396.0 (CEF), m/z172.2→m/z 128.2 (MET), m/z188.0→m/z125.9 (MET-OH) and m/z528.1→m/z 364.0 (CEFU) to quantify the drugs. Calibration curves in spiked plasma and ultra-filtrate were linear (r2 ≥ 0.9948) from 0.4–300 µg/mL for CEF, 0.05–50 µg/mL for MET and 0.02 – 30 µg/mL for MET-OH. The intra- and inter- assay precisions were less than 9% and the mean extraction recoveries were 94.0% (CEF), 98.2% (MET), 99.6% (MET-OH) and 104.6% (CEF in ultra-filtrate); the recoveries for the IS were 93.8% (in plasma) and 97.6% (in ultra-filtrate). The validated method was successfully applied to a pharmacokinetic study of CEF, MET and MET-OH in hospitalized children with complicated severe acute malnutrition following an oral administration of MET and intravenous administration of CEF over the course of 72 hours.

scholarly journals Development, Validation, and Routine Application of a High-Performance Liquid Chromatography Method Coupled with a Single Mass Detector for Quantification of Itraconazole, Voriconazole, and Posaconazole in Human Plasma

2010 ◽  
Vol 54 (8) ◽  
pp. 3408-3413 ◽  
Author(s):  
Lorena Baietto ◽  
Antonio D'Avolio ◽  
Giusi Ventimiglia ◽  
Francesco Giuseppe De Rosa ◽  
Marco Siccardi ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Internal Standard ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
True Value ◽  
Relative Standard ◽  
Mass Detector ◽  
Liquid Chromatography Method

ABSTRACT We have developed and validated a high-performance liquid chromatography method coupled with a mass detector to quantify itraconazole, voriconazole, and posaconazole using quinoxaline as the internal standard. The method involves protein precipitation with acetonitrile. Mean accuracy (percent deviation from the true value) and precision (relative standard deviation percentage) were less than 15%. Mean recovery was more than 80% for all drugs quantified. The lower limit of quantification was 0.031 μg/ml for itraconazole and posaconazole and 0.039 μg/ml for voriconazole. The calibration range tested was from 0.031 to 8 μg/ml for itraconazole and posaconazole and from 0.039 to 10 μg/ml for voriconazole.

scholarly journals Determination of Intact Parabens in the Human Plasma of Cancer and Non-Cancer Patients Using a Validated Fabric Phase Sorptive Extraction Reversed-Phase Liquid Chromatography Method with UV Detection

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1526
Author(s):  
Anthi Parla ◽  
Eirini Zormpa ◽  
Nikolaos Paloumpis ◽  
Abuzar Kabir ◽  
Kenneth G. Furton ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Reversed Phase ◽  
Plasma Samples ◽  
Reversed Phase Liquid Chromatography ◽  
Chromatography Method ◽  
Sorptive Extraction ◽  
Human Plasma Samples ◽  
Phase Liquid ◽  
Liquid Chromatography Method

Parabens have been widely employed as preservatives since the 1920s for extending the shelf life of foodstuffs, medicines, and daily care products. Given the fact that there are some legitimate concerns related to their potential multiple endocrine-disrupting properties, the development of novel bioanalytical methods for their biomonitoring is crucial. In this study, a fabric phase sorptive extraction reversed-phase liquid chromatography method coupled with UV detection (FPSE-HPLC-UV) was developed and validated for the quantitation of seven parabens in human plasma samples. Chromatographic separation of the seven parabens and p-hydroxybenzoic acid was achieved on a semi-micro Spherisorb ODS1 analytical column under isocratic elution using a mobile phase containing 0.1% (v/v) formic acid and 66% 49 mM ammonium formate aqueous solution in acetonitrile at flow rate 0.25 mL min−1 with a 24-min run time for each sample. The method was linear at a concentration range of 20 to 500 ng mL−1 for the seven parabens under study in human plasma samples. The efficiency of the method was proven with the analysis of 20 human plasma samples collected from women subjected to breast cancer surgery and to reconstructive and aesthetic breast surgery. The highest quantitation rates in human plasma samples from cancerous cases were found for methylparaben and isobutylparaben with average plasma concentrations at 77 and 112.5 ng mL−1. The high concentration levels detected agree with previous findings for some of the parabens and emphasize the need for further epidemiological research on the possible health effects of the use of these compounds.

scholarly journals Method development and validation of amlodipine and cilnidipine in human plasma by using liquid chromatography and tandem mass spectrometry

2021 ◽  
Vol 12 (1) ◽  
pp. 620-630
Author(s):  
Muni Krishnaiah A ◽  
Rama Chandraiah C ◽  
Srinivas M ◽  
Devanna N
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Method Development ◽  
Stationary Phases ◽  
Internal Standard ◽  
Reversed Phase ◽  
Detection Sensitivity ◽  
Tandem Mass

Amlodipine and Cilnidipine in K2EDTA plasma were determined by Liquid Chromatography and Tandem Mass Spectrometry. To improve LC separation and detection sensitivity for the LC-MS technique interface of contiguous stationary phases and LC gradients were enhanced. For separation Acetonitrile was used as eluent. Reversed phase C8 and C18, X-bridge columns were utilized. Telmisartan was used an Internal Standard in this process. For elution Telmisartan needs acidic PH but Amlodipine and Cilnidipine needs neutral PH, dilution with H2O for supernate get afterward extraction. The standards were separated in existence of Telmisartan as internal standard from Amlodipine and Cilnidipine by LC-MS/MS using the MRM transitions. The extracted ion chromatograms were considered from peak ratio of analyte to internal standard. Human plasma without analytes, and solutions containing analytes without human plasma were also analysed. To determine the stability analyte was kept in steady state at room temperature for 24 hrs in plasma. The instrument had operating in positive ion mode. The product ion mass spectra of Amlodipine were 409.1→237.7 and Cilnidipine was 493.2 →117.1. Quadratic regression was used to generate calibration curve by the Analyst 1.5 software program. To obtain the linear response the concentration range is 1-1000ng/mL. For each analyte intra (n=6/batch, 3 days) and inter-batch (n=18) accuracy and precision values were obtained.

scholarly journals Liquid chromatography–tandem mass spectrometry for the simultaneous quantitation of ceftriaxone, metronidazole and hydroxymetronidazole in plasma from seriously ill, severely malnourished children

2018 ◽  
Vol 2 ◽  
pp. 43 ◽  
Author(s):  
Martin Ongas ◽  
Joseph Standing ◽  
Bernhards Ogutu ◽  
Joseph Waichungo ◽  
James A. Berkley ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Severe Acute Malnutrition ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Reversed Phase ◽  
Cefuroxime Axetil ◽  
Acute Malnutrition ◽  
Ionization Mass ◽  
Chromatography Method

We have developed and validated a novel, sensitive, selective and reproducible reversed-phase high-performance liquid chromatography method coupled with electrospray ionization mass spectrometry (HPLC–ESI-MS/MS) for the simultaneous quantitation of ceftriaxone (CEF), metronidazole (MET) and hydroxymetronidazole (MET-OH) from only 50 µL of human plasma, and unbound CEF from 25 µL plasma ultra-filtrate to evaluate the effect of protein binding. Cefuroxime axetil (CEFU) was used as an internal standard (IS). The analytes were extracted by a protein precipitation procedure with acetonitrile and separated on a reversed-phase Polaris 5 C18-Analytical column using a mobile phase composed of acetonitrile containing 0.1% (v/v) formic acid and 10 mM aqueous ammonium formate pH 2.5, delivered at a flow-rate of 300 µL/min. Multiple reaction monitoring was performed in the positive ion mode using the transitions m/z555.1→m/z396.0 (CEF), m/z172.2→m/z 128.2 (MET), m/z188.0→m/z125.9 (MET-OH) and m/z528.1→m/z 364.0 (CEFU) to quantify the drugs. Calibration curves in spiked plasma and ultra-filtrate were linear (r2 ≥ 0.9948) from 0.4–300 µg/mL for CEF, 0.05–50 µg/mL for MET and 0.02 – 30 µg/mL for MET-OH. The intra- and inter- assay precisions were less than 9% and the mean extraction recoveries were 94.0% (CEF), 98.2% (MET), 99.6% (MET-OH) and 104.6% (CEF in ultra-filtrate); the recoveries for the IS were 93.8% (in plasma) and 97.6% (in ultra-filtrate). The validated method was successfully applied to a pharmacokinetic study of CEF, MET and MET-OH in hospitalized children with complicated severe acute malnutrition following an oral administration of MET and intravenous administration of CEF over the course of 72 hours.

Determination of trigonelline in human plasma by magnetic solid-phase extraction: a pharmacokinetic study

Nanomedicine ◽  
2021 ◽  
Vol 16 (4) ◽  
pp. 323-333
Author(s):  
Neda Mohamadi ◽  
Fariba Sharififar ◽  
Mostafa Pournamdari ◽  
Mehdi Ansari
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Solid Phase ◽  
Reversed Phase ◽  
Dose Finding ◽  
Plasma Samples ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Aim: To develop a novel method for the bioanalytical extraction of trigonelline (TRG) from human plasma samples using a magnetic nanocomposite and to evaluate its pharmacokinetic profile. Materials & methods: Magnetic bentonite/β-cyclodextrine (β-CD) nanoparticles, coupled with a validated ion-pairing reversed-phase high-performance liquid chromatography method, were used to determine TRG concentration from plasma samples following a single oral administration. Results: The developed reversed-phase high-performance liquid chromatography method was accurate, precise, specific, selective and reproducible. TRG showed rapid absorption, middle rate of elimination and mean residence time of ∼24 h. The data were best fitted on a two-compartment model in which tmax was 1.0 h, Cmax 0.115 μg/ml, area under the curve (AUC)0–24 1.72 μg/ml.h, Cl 0.0293 l/h/kg, t1/2α 0.79 h, t1/2β 13.68 h and ka 1.63 h-1. Conclusion: The findings of this study could provide useful information to promote the future study of TRG and aid optimal dose finding.

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