scholarly journals Simultaneous determination of three naphthoquinones from Arnebia euchroma (Royle) Johnst in beagle plasma by UPLC-MS/MS and application for pharmacokinetics study

2021 ◽  
Keyword(s):  
Electrospray Ionization ◽  
Simultaneous Determination ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Limit Of Quantification ◽  
Arnebia Euchroma ◽  
Validation Parameters ◽  
Negative Ionization Mode ◽  
Negative Ionization

Abstract A rapid, simple and efficient ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was established to simultaneous determination of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle plasma and evaluated by using esculetin as internal standard. The electrospray ionization (ESI) source was operated in negative ionization mode. Multi-reaction monitoring (MRM) was used to quantitatively analyzed shikonin m/z 287.0 → 217.9, isobutyryl shikonin m/z 357.0 → 268.9, β, βʹ-dimethylacryl alkanin m/z 370.0 → 270.1 and esculetin m/z 177.0 → 89.0, respectively. The method was validated for selectivity, linearity, lower limit of quantification, precision, accuracy, recovery, matrix effect and stability. All validation parameters met the acceptance criteria according to regulatory guidelines. This method was successfully applied for the pharmacokinetic study of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle dogs plasma after oral administration of A. euchroma extract.

scholarly journals UPLC–MS/MS simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, MDMA, and MDA in hair

2020 ◽  
Vol 32 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Peiwu Geng
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Ammonium Hydroxide ◽  
Ultra Performance Liquid Chromatography ◽  
Acetate Solution ◽  
Hair Samples ◽  
Relative Standard

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.

scholarly journals Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization

2015 ◽  
Vol 65 (2) ◽  
pp. 159-169 ◽  
Author(s):  
Paweł Szpot ◽  
Grzegorz Buszewicz
Keyword(s):  
Electrospray Ionization ◽  
Human Plasma ◽  
Ultra Performance Liquid Chromatography ◽  
High Accuracy ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Flight Mass Spectrometry ◽  
Tof Ms ◽  
Chemical Formulas

Abstract This report presents the application of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry with positive electrospray ionization, to determine ramipril in human plasma. First, the proteins in human plasma were precipitated using acetonitrile, then the supernatant was extracted by ethyl acetate at pH 3 and finally, the extract was analyzed using a UPLC-QTOF- MS system. The method was validated and the coefficient of determination (R2) was > 0.999, the lower limit of quantification (LLOQ) was 0.5 ng mL-1. Precision, recovery and stability were determined for three different concentrations of ramipril. RSD for this method ranged from 3.3 to 8.6 %. The intra-day mean recovery was from 65.3 to 97.3 %. In addition, the fragmentation of ramipril was studied. Due to high resolution of the spectrometer, it was possible to measure fragment masses accurately and determine their molecular and chemical formulas with high accuracy.

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.

Rapid simultaneous determination of herbicides in human serum by UPLC-ESI-MS

2014 ◽  
Vol 6 (17) ◽  
pp. 6939-6947 ◽  
Author(s):  
Xinfeng Dong ◽  
Zhihong Shi ◽  
Shuxuan Liang ◽  
Hanwen Sun
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Serum ◽  
Electrospray Ionization ◽  
Simultaneous Determination ◽  
Electrospray Ionization Mass Spectrometry ◽  
Reliable Method ◽  
Ultra Performance Liquid Chromatography ◽  
Ionization Mass

A simple, rapid and reliable method is developed for the determination of 51 kinds belonging to at least 8 classes of herbicides in human serum by ultra performance liquid chromatography-electrospray ionization-mass spectrometry.

scholarly journals Simultaneous Determination of Rofecoxib and Tizanidine by HPTLC

2009 ◽  
Vol 6 (1) ◽  
pp. 295-302 ◽  
Author(s):  
Uttam D. Pawar ◽  
Aruna V. Sulebhavikar ◽  
Abhijit V. Naik ◽  
Satish G. Pingale ◽  
Kiran V. Mangaonkar
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Volume Ratio ◽  
Standard Addition ◽  
Limit Of Quantification ◽  
Chromatography Method

An innovative high performance thin layer chromatography method was developed and validated for simultaneous determination of rofecoxib and tizanidine from tablet dosage form. Rosiglitazone maleate was used as an internal standard. The separation was achieved using HPTLC plates (Merck #5548) precoated with silica gel 60F254on aluminum sheets and a mobile phase comprising of toluene: ethyl acetate: methanol: triethyl amine in volume ratio of 6:3:0.5:0.1 (v/v/v/v), with chamber saturation of 15 min. The plate was developed up to 8 cm and air dried. The plate was then scanned and quantified at 235 nm. The linearity of rofecoxib and tizanidine were in the range of 3.75 µg/spot to 11.25 µg/spot and 0.30 µg/spot to 0.90 µg/spot respectively. The limit of detection for rofecoxib and tizanidine was found to be 45.00 ng/spot and 30.00 ng/spot respectively. The limit of quantification for rofecoxib and tizanidine was found to be 135.00 ng/spot and 90.00 ng/spot respectively. The percentage assay was found between the range of 99.58% to 103.21% for rofecoxib and 98.73% to 101.55% for tizanidine respectively, whereas recovery was found between 99.97% to 100.43% for rofecoxib and 100.00% to 101.00% for tizanidine by standard addition method. The proposed method is accurate, precise and rapid for the simultaneous determination of rofecoxib and tizanidine in dosage form

scholarly journals Development and validation of an improved HPLC-UV method for simultaneous determination of lamotrigine and oxcarbazepine and its active metabolite 10,11-dihydro-10-hydroxycarbazepine in human blood plasma and comparison with an UHPLC-MS/MS method

2019 ◽  
Vol 10 (1) ◽  
Author(s):  
Siyao Jin ◽  
Qing Zhao ◽  
Dongjie Zhang ◽  
Zhigang Zhao ◽  
Shenghui Mei
Keyword(s):  
Liquid Chromatography ◽  
Blood Plasma ◽  
Simultaneous Determination ◽  
Human Blood ◽  
High Performance ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Human Blood Plasma ◽  
Elution Time

AbstractLamotrigine (LTG) and oxcarbazepine (OXC) are first-line drugs for epilepsy treatment. Their large pharmacokinetics variabilities and relations between efficacy and toxicity and blood plasma concentration require routine monitoring for dose adjustment. In this study, we developed and validated a simple, accurate, and reliable method for simultaneous determination of LTG, OXC and 10,11-dihydro-10-hydroxycarbazepine (MHD) in human blood plasma by high-performance liquid chromatography-ultraviolet detection (HPLC-UV) with a simple one-step protein precipitation using methanol (1% acetic acid) and 15 min elution time under isocratic elution at 1 mL/min. Calibration range was 2.4 to 120 mg/L for LTG, OXC, and MHD. The intra-day and inter-day bias were − 8.84 to 4.18%, and the imprecision was less than 8.08% for all analytes. The internal standard (fluconazole) normalized recovery was 96.30 to 107.69% for LTG, 98.51 to 111.04% for MHD, and 95.04 to 109.86% for OXC. A total of 186 LTG samples and 25 MHD samples were used to evaluate the agreement between HPLC-UV and ultra-performance liquid chromatography-mass spectrometry (UHPLC-MS/MS) by Passing-Bablok regression and Bland-Altman plot. The mean bias and the 95% limits of agreement (95% LOA) of the two measurements were 0.575 mg/L and − 1.238 to 2.387 mg/L for LTG (n = 186) and − 1.222 mg/L and − 8.271 to 5.827 mg/L for MHD (n = 25), which indicated the UV method was comparable with the MS method for LTG and MHD analysis.

A UPLC-MS/MS Method for Simultaneous Determination of Six Bioactive Compounds in Rat Plasma, and its Application to Pharmacokinetic Studies of Naoshuantong Granule in Rats

2019 ◽  
Vol 15 (3) ◽  
pp. 231-242
Author(s):  
Ping Wang ◽  
Shenmeng Jiang ◽  
Yu Zhao ◽  
Shuo Sun ◽  
Xiaoli Wen ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Negative Ion ◽  
Pharmacokinetic Studies ◽  
Acquity Uplc

Background: It is urgently needed to clarify the pharmacokinetic mechanism for the multibioactive constituents in Traditional Chinese Medicines for its clinical applications. A rapid, sensitive and reliable ultra-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of Danshensu, Ferulic acid, Astragaloside IV, Naringin, Neohesperidin and Puerarin after oral administration of Naoshuantong Granule using Carbamazepine as internal standard (IS). Methods: The plasma samples were pretreated by liquid-liquid extraction method using ethyl acetate after acidification, and separated on a Waters ACQUITY UPLC® BEH C18 column (50×2.1 mm, i.d., 1.7 µm) by gradient elution with a mobile phase composing of water (containing 0.1% formic acid) and acetonitrile at a flow rate of 0.2 mL/min. Multiple reaction monitoring (MRM) mode with both positive and negative ion mode was operated using an electrospray ionization (ESI) to detect the six compounds. Result: All calibration curves showed good linearity (r>0.99) over a wide concentration range. The intra- and inter-day precision (RSD%) was below 8.4% and the accuracy (RE%) ranged from 91.1% to 107.5%. The extraction recoveries of the six analytes and IS in the plasma were more than 77.9% and no severe matrix effect was observed. Conclusion: The fully validated method was successfully applied to the pharmacokinetics of Naoshuantong Granule.

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