scholarly journals Development and Validation of an HPLC/MS/MS Method for Determining the Thiazolidinone PG15 in Rat Plasma

2010 ◽  
Vol 93 (4) ◽  
pp. 1215-1221
Author(s):  
FláVia D T UchôA ◽  
Eduardo C Palma ◽  
Natalia F Souza ◽  
Maria C A Lima ◽  
Suely L Galdino ◽  
...  
Keyword(s):  
Internal Standard ◽  
Ammonium Hydroxide ◽  
Rat Plasma ◽  
Negative Ion ◽  
Pharmacokinetic Studies ◽  
Plasma Samples ◽  
Isocratic Elution ◽  
Negative Ion Mode ◽  
Development And Validation

Abstract A rapid, sensitive, and simple HPLC/MS/MS method was developed and validated for the determination of (5Z,E)-3-[2-(4-chlorophenyl)-2-oxoethyl]-5-(1H-indol-3-ylmethylene)-thiazolidine-2, 4-dione (PG15) in rat plasma using chlortalidone as an internal standard (IS). Analyses were performed using a C18 column and isocratic elution with acetonitrilewater (90 + 10, v/v) containing 10 mM ammonium hydroxide (pH 8.0) as the mobile phase pumped at 0.3 mL/min. Detection was performed by MS with negative ion mode electrospray ionization. Rat plasma samples were prepared by deproteinizing with acetonitrile. Detected fragments were 395.1 > 171.9 for PG15 and 337.3 > 189.9 for the IS. Calibration curves were linear from 10 to 1000 ng/mL, with the determination coefficient >0.99. The intraday and interday precisions were less than 12.2 and 11.3, respectively. The applicability of the HPLC/MS/MS method for pharmacokinetic studies was tested using plasma samples obtained after oral administration of PG15 to rats, and it provided the necessary sensitivity, linearity, precision, accuracy, and specificity.

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.

Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Canagliflozin and Metformin HCl in Rat Plasma and its Application

2020 ◽  
Vol 16 (6) ◽  
pp. 752-762
Author(s):  
Vivek Nalawade ◽  
Vaibhav A. Dixit ◽  
Amisha Vora ◽  
Himashu Zade
Keyword(s):  
Internal Standard ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Herbal Extracts ◽  
One Step ◽  
Precision And Accuracy ◽  
Development And Validation ◽  
The Impact ◽  
Metformin Hcl

Background: Food and herbal extracts rich in Quercetin (QRT) are often self-medicated by diabetics and can potentially alter the pharmacokinetics (PK) of Metformin HCl (MET) and Canagliflozin (CNG) leading to food or herb-drug interactions and reduced therapeutic efficacy. However, the impact of these flavonoids on the pharmacokinetic behaviour of MET and CNG is mostly unknown. Methods: A simple one-step protein precipitation method was developed for the determination of MET and CNG from rat plasma. The mobile phase chosen was MeOH 65% and 35% water containing 0.1% formic acid at a flow rate of 1mL/min. Results: The retention time of MET, internal standard (Valsartan) and CNG was 1.83, 6.2 and 8.2 min, respectively. The method was found to be linear in the range of 200 - 8000 ng/mL for CNG and 100 = 4000 ng/ml for MET. Precision and accuracy of the method were below 20% at LLOQ and below 15% for LQC, MQC, and HQC. Conclusion: The method was successfully applied for the determination of PK of MET and CNG by using 100 μL of rat plasma. QRT co-administration affects the PK parameters of MET and CNG. This alteration in PK parameters might be of significant use for clinicians and patients.

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.

A Novel LC-MS Method for the Determination of Abiraterone in Rat Plasma and its Application to Pharmacokinetic Studies

2021 ◽  
Vol 17 ◽  
Author(s):  
Linzhi Dai ◽  
Pei Lv ◽  
Yun He ◽  
Xiaoli Wang ◽  
Lili Chen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Rat Plasma ◽  
Pharmacokinetic Studies ◽  
Quadrupole Mass ◽  
Limit Of Quantitation

Background: High–performance liquid chromatography (HPLC)–ultraviolet (UV) and liquid chromatography (LC)–mass spectrometry (MS)/MS methods have been used to analyse abiraterone (ART); however, a single-quadrupole mass spectrometer with LC-MS systems has never been used to analyse ART. Objective: The study aimed to establish a novel, simple assay of quantitating ART in rat plasma through LC–MS. Method: The analytical procedure involved the extraction of ART and D4-ART (internal standard, IS) from rat plasma through simple protein precipitation. Chromatographic separation was achieved using an isocratic mobile phase (acetonitrile: 5 mM ammonium formate with 0.1% formic acid, 50:50 v/v) at a flow rate of 0.30 mL/min on a Waters XBridge® C18 column with a total run time of 5 min. LC–MS ion transitions monitored were 350.1 and 354.1 for ART and IS, respectively. The method was validated, and the results met acceptance criteria. Results: The lower limit of quantitation achieved was 1 ng/mL, and linearity was 1–8000 ng/mL. The intra- and inter-day precisions were 1.26%–14.20% and 5.49%–13.08%, respectively, in rat plasma.

A HPLC-DAD-MS/MS Method for Simultaneous Determination of Six Active Ingredients of Salviae Miltiorrhizae and Ligustrazine Hydrochloride Injection in Rat Plasma and its Application to Pharmacokinetic Studies

2020 ◽  
Vol 21 ◽  
Author(s):  
Jianyang Pan ◽  
Luquan Zhang ◽  
Difeifei Xiong ◽  
Bailing Li ◽  
Haibin Qu
Keyword(s):  
Simultaneous Determination ◽  
Pharmacokinetic Study ◽  
Rat Plasma ◽  
Array Detector ◽  
Pharmacokinetic Studies ◽  
Plasma Samples ◽  
Active Ingredients ◽  
Salviae Miltiorrhizae ◽  
Salvianolic Acids

Aims: Pharmacokinetic Study of Salviae Miltiorrhizaeand Ligustrazine Hydrochloride injection. For the evaluation of mechanism of action, safety and clinical rational use of Salviae Miltiorrhizae and Ligustrazine Hydrochloride injection. Background: Salviae Miltiorrhizae and Ligustrazine Hydrochloride injection is a compound preparation consisted of Salvia Miltiorrhiza extract and ligustrazine hydrochloride for the treatment of cardiovascular and cerebrovascular diseases in China. Methods: Plasma samples were precipitated with methanol, which was spiked with ascorbic acid and the supernatant was separated on a Waters Cortecs C18 column, by using a gradient mobile phase system of acetonitrile-water containing 0.05% formic acid (v/v). For internal standards, puerarin was selected for the five salvianolic acids, while isofraxidin was used for ligustrazine hydrochloride. Besides, electrospray ionization in negative mode and multiple-reaction monitoring were used to identify and quantify the five salvianolic acids, whereas ligustrazine hydrochloride was quantified at 310 nm using the diode array detector. Results: Noticeably, all calibration curves showed good linearity (R2>0.99) over the concentration range, with a lower limit of quantification between 0.00411 and 0.0369μg/mL for salvianolic acids, and 1.74 μg/mL for ligustrazine hydrochloride. Next, the precision of the developed method was evaluated by intra-and inter-day assays, and the percentage of relative standard deviation was within 10%. Although the extraction efficiency of some salvianolic acids were not very satisfactory, the sensitivity of the analytical method met the analysis requirements of rat plasma samples. Moreover, the validated method was successfully applied to a pharmacokinetic study of Salviae Miltiorrhizae and Ligustrazine Hydrochloride injection in the rat model. Conclusion: Linear pharmacokinetic characteristics were observed for the six active ingredients after intravenous infusion administration in rats, within the dose range examined here. In summary, our study proposed a HPLC-DAD-MS/MS method in the simultaneous determination of multiple ingredients, and demonstrated its applicability in pharmacokinetic studies.

Simultaneous determination of pentoxifylline and three metabolites in biological fluids by liquid chromatography.

1989 ◽  
Vol 35 (2) ◽  
pp. 298-301 ◽  
Author(s):  
W E Lambert ◽  
M A Yousouf ◽  
B M Van Liedekerke ◽  
J E De Roose ◽  
A P De Leenheer
Keyword(s):  
Acetic Acid ◽  
Liquid Chromatography ◽  
Hydrochloric Acid ◽  
Simultaneous Determination ◽  
Biological Fluids ◽  
Internal Standard ◽  
Pharmacokinetic Studies ◽  
Plasma Samples ◽  
Liquid Chromatographic

Abstract We describe a sensitive and specific liquid-chromatographic assay for pentoxifylline and three of its metabolites in human plasma and urine. Addition of hydrochloric acid to the sample before extraction, and incorporation of acetic acid in the chromatographic eluent, allow the simultaneous determination of the four compounds plus an internal standard in one chromatographic run. Unlike gas-chromatographic procedures, this method does not involve derivatization no similar analysis of serum or plasma samples has been described before now. The method has been applied successfully to routine analysis and to pharmacokinetic studies.

scholarly journals Comparative pharmacokinetic study of five flavonoids in normal rats and rats with gastric ulcer following oral administration of Mongolian medicine, Shudage - 4 by UPLC – ESI – MS/MS

2020 ◽  
Vol 19 (3) ◽  
pp. 651-659
Author(s):  
Xin Jia ◽  
Yinfei Du ◽  
Jia Xu ◽  
Yu Dong
Keyword(s):  
Gastric Ulcer ◽  
Oral Administration ◽  
Internal Standard ◽  
Rat Plasma ◽  
Negative Ion ◽  
Selected Reaction Monitoring ◽  
Pharmacokinetic Parameters ◽  
Ionization Mass ◽  
Plasma Samples ◽  
Esi Ms

Purpose: To develop a simple, rapid and sensitive ultra-performance liquid chromatography - electrospray ionization-mass spectrometry (UPLC–ESI–MS/MS) method was developed and fully validated for the simultaneous determination of galangin, kaempferide, galangin-3-methylether, kaempferol and quercetin in rat plasma after oral administration of Mongolian Medicine, Shudage-4 extracts. Methods: The galangin, kaempferide, galangin-3-methylether, kaempferol and quercetin were separated on a C18 column using 0.1 % formic acid at a flow rate of 0.4 mL / min and detected by a mass spectrometer in negative-ion mode with selected reaction monitoring (SRM) mode. Plasma samples were processed with a simple deproteinization technique using ethyl acetate and acetonitrile. Following the protein precipitation, the plasma samples were evaporated under gentle stream of nitrogen and analyzed by above method. Naringin was used as an internal standard (IS). Method validation was performed according to the Chinese Food and Drug Administration guidelines. Results: A good linearity (r2 ≥ 0.9990) was showed by the UPLC – ESI – MS / MS method, the low limits of quantification for galangin, kaempferide, galangin-3-methylether, kaempferol and quercetin were 229.8, 78.8, 32.0, 123.7 and 137.8 ng / mL, respectively. The results of inter-day and intra-day precisions met the experimental requirement (< 7.8 %). The matrix effect and recovery efficiency of the five analytes were more than 72.9 and 88.7 % respectively. The stability of the analytes were satisfactory. The UPLC – ESI – MS / MS method has been used for the five analytes’ pharmacokinetics study successfully after gastrointestinal route of the Mongolian Medicine Shudage-4. The pharmacokinetic parameters showed significant differences (P < 0.05) between the normal and gastric ulcer groups. The metabolism and transport of the five analytes in gastric ulcer rates were faster than in normal rats after administration of Shudage - 4 extract. Double-peak phenomenon appeared in galangin, galangin – 3 - methylether and quercetin. Conclusion: The results suggest that the metabolism and transport of Mongolian Medicine Shudage-4 in gastric ulcer rats is faster than in normal rats and may be enriched and acted on at the lesion site. Keywords: UPLC – ESI – MS / MS; Mongolian medicine; Shudage - 4; pharmacokinetics; gastric ulcer

scholarly journals Development and Validation of Ultra High Performance Liquid Chromatographic (UHPLC) Method for the Determination of Roxithromycin in the Broiler Plasma

2019 ◽  
pp. 1-8
Author(s):  
R. D. Singh ◽  
S. K. Mody ◽  
H. B. Patel ◽  
V. N. Sarvaiya ◽  
B. R. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Pharmacokinetic Studies ◽  
Uv Detector ◽  
Linear Calibration ◽  
The Mean ◽  
Development And Validation ◽  
Liquid Chromatographic

Aims: The present study was designed to develop and validate the UHPLC method for quantitative determination of roxithromycin, a macrolide antimicrobial drug, in broiler plasma for the application of pharmacokinetic studies. Methodology: UHPLC apparatus comprised of ultraviolet (UV) detector was used in the present study. Chromatographic separation was performed by using reverse phase C18 column. Mobile phase was combination of buffer and 55 acetonitrile in the ratio of 55: 45. Buffer part used was 0.1% trifluoroacetic acid (v/v) having pH of 2.1. Erythromycin was used as an internal standard. Isocratic elution mode was employed with flow rate of 1 ml/min and effluents were monitored at wavelength of 220 nm. Liquid-liquid extraction using ice-cold acetonitrile was performed to extract roxithromycin from plasma samples. The data integration was performed using Chromeleon™ version 6.8 software. Results: The linear calibration curve with a mean correlation coefficient (R2) value of 0.9999 was observed for concentrations ranging from 0.20 to 12.80 µg/ml. At any concentration, accuracy was not found to be less than 90%. The mean extraction recovery (n=5) for concentrations of 0.40 µg/ml was 81.36%. The calculated intraday and interday C.V. % was not more than 7.70% and 9.42%, respectively, at any concentration studied. The specificity of the analysis was reflected by the narrow range of retention time ranging between 6.983 to 7.178 minutes. LOD and LOQ of the method under investigation were calculated as 0.131 and 0.398 µg/ml, respectively. Conclusion: A reliable, reproducible, accurate, precise, specific and sensitive method for analysis of roxithromycin in broiler plasma was developed and validated for application in the pharmacokinetic study of the roxithromycin.

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