Determination and validation of aprepitant in rat plasma using LC−MS/MS

Bioanalysis ◽  
2021 ◽  
Vol 13 (5) ◽  
pp. 363-372
Author(s):  
Nazlı Erdoğar ◽  
Tuba Reçber ◽  
Alper B İskit ◽  
Erem Bilensoy ◽  
Sedef Kır ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Formic Acid ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Pharmacokinetic Parameters ◽  
Reaction Monitoring ◽  
Bioanalytical Method Validation ◽  
Bioanalytical Method ◽  
Acceptable Range ◽  
Multiple Reaction Monitoring Mode

Aim: The assessment of efficacy should be paralleled with extensive pharmacokinetic parameters, and a valid bioanalytical method is a pre-condition for accurate plasma concentration. Materials & methods: A simple, specific, rapid and sensitive LC−MS/MS method has been developed for quantitative analysis of aprepitant in rat plasma. A C18 column was used as stationary phase and the mobile phase consisted of a mixture of formic acid in water and formic acid in acetonitrile. Quantification was performed using multiple reaction monitoring mode. Results: The selectivity, linearity, accuracy, precision, robustness and ruggedness of the method were evaluated in accordance with bioanalytical method validation guideline of ICH and all results were within the acceptable range. Conclusion: The validated LC−MS/MS method was found to be useful for the quantitative analysis of aprepitant in rat plasma samples.

Quantification and confirmation of four aflatoxins using a LC–MS/MS QTRAP system in multiple reaction monitoring, enhanced product ion scan, and MS3 modes

2019 ◽  
Vol 26 (1) ◽  
pp. 63-77
Author(s):  
Shencong Lv ◽  
Henghui Wang ◽  
Yong Yan ◽  
Miaohua Ge ◽  
Jian Guan
Keyword(s):  
Formic Acid ◽  
Ion Trap ◽  
Multiple Reaction Monitoring ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Reaction Monitoring ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Derivative Products

A simple, rapid, and efficient liquid chromatography tandem mass spectrometry (LC–MS/MS) method, operated in electrospray ionization and quadrupole linear ion trap modes, has been developed for the identification and structural characterization of aflatoxins in peanuts and its derivative products or bean sauce. Samples (5 g) were extracted with acetonitrile/water/formic acid (79:20:1, v/v). After centrifugation and dilution, the extracts were separated on a C18 analytical column by gradient elution (acetonitrile/0.2% formic acid) and analyzed by UPLC–MS/MS. External calibration was used for qualification. The developed multiple reaction monitoring–information-dependent acquisition–enhanced product ion method enabled quantification and confirmation of the analytes in a single run. Enhanced product ion mode was used for qualitative analysis, while multiple reaction monitoring mode was used for quantitative analysis. An in-house library was constructed for identification. Calibration curves showed good linearity with correlation coefficients (r) higher than 0.994. Limits of detection were determined to be below 0.26 µg kg−1 for most analytes. The recoveries for those substances were in the acceptable range of 80.2%–119.1%. A new LC–MS3 method was established for further confirmation. One pickled pepper peanut was found to contain aflatoxins B1, B2, and G1 with contents of 90.93, 26.64, and 1.92 µg kg−1, respectively.

A Comparative Pharmacokinetic Study of Schisandrol B After Oral Administration of Schisandrol B Monomer and Schisandra chinensis Extract

2019 ◽  
Vol 16 ◽  
Author(s):  
Zijing Wu ◽  
Dahu Liang ◽  
Maodi Xu ◽  
Yanhao Liu ◽  
Haitang Xie
Keyword(s):  
Oral Administration ◽  
Formic Acid ◽  
Multiple Reaction Monitoring ◽  
The Body ◽  
Methyl Tert Butyl Ether ◽  
Pharmacokinetic Parameters ◽  
Schisandra Chinensis ◽  
Sprague Dawley ◽  
Butyl Ether ◽  
Multiple Reaction Monitoring Mode

Background: Schisandra chinensis Turcz. (Baill.) is a perennial deciduous woody vine plant that is beneficial to all systems of the body. Objective: The goals of the present study were to compare the pharmacokinetics of schisandrol B in rats after oral administration of schisandrol B monomer (10 mg/kg) and S. chinensis extract (equivalent to 10 mg/kg schisandrol B) and to explore interactions among the components in S. chinensis extract. Method: Twelve Sprague-Dawley rats of SPF grade were randomly divided into the monomer and S.chinensis extract groups. Plasma samples were extracted with methyl tert-butyl ether, and chromatographic separation was performed on an Agilent ZORBAX Eclipse XDB-C18 (4.6 × 150 mm, 5 μm) column with the mobile phase consisting of methanol (containing 0.1% formic acid)-water (containing 0.1% formic acid and 5 mmol ammonium acetate). This analysis was achieved by multiple reaction monitoring mode in an electrospray interface. Results: The seven lignans had good linear relationship within the determination range (r>0.9950); the intra- and inter-day precision were < 12.08% and accuracy was 88.64%-111.61%. The pharmacokinetic parameters (T1/2, Tmax, MRT0-∞, CL, AUC0-t, and AUC0-∞) of schisandrol B showed significant differences between the two groups (P < 0.05). Conclusion: The validated method has been successfully applied to the pharmacokinetics of schisandrin, schisandrol B, schisandrin A, schisandrin B, schisandrin C, schisanhenol, and schisantherin A. The pharmacokinetic differences indicate that other components in the extract may increase the absorption of schisandrol B, decrease the rate of elimination, and improve the bioavailability of schisandrol B.

scholarly journals Development and Validation of UPLC-MS/MS Method for Determination of Enasidenib in Rat Plasma and Its Pharmacokinetic Application

2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Shuang-long Li ◽  
Yong-liang Zhu ◽  
Yi Zhang ◽  
Shu-han Liu ◽  
Xiang-die Wang ◽  
...  
Keyword(s):  
Mass Transfer ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Bioanalytical Method Validation ◽  
Fda Approval ◽  
Elution Method ◽  
Acquity Uplc ◽  
Development And Validation

In our research, a straightforward UPLC-MS/MS method, with diazepam as the internal standard (IS), was proposed and acknowledged to determine the concentrations of enasidenib in rat plasma. When preparing the sample, we used acetonitrile for protein precipitation. The gradient elution method was used, and the mobile phase was acetonitrile and 0.1% formic acid. Diazepam was used as the IS. We used the Acquity UPLC BEH C18 column to separate enasidenib and IS. Under the positive ion electrospray ionization (ESI) source conditions, the mass transfer pairs of enasidenib were monitored by multiple reaction monitoring (MRM) to be m/z 474.2 ⟶ 456.1 and m/z 474.2 ⟶ 267.0, and the IS mass transfer pairs were m/z 285.0 ⟶ 154.0. Enasidenib had good linearity (r2 = 0.9985) in the concentration range of 1.0–1000 ng/mL. Besides, the values of intraday and interday precision were 2.25–8.40% and 3.94–5.46%, respectively, and the range of the accuracy values varied from −1.44 to 2.34%. Matrix effect, extraction recovery, and stability were compliant with FDA approval guidelines in terms of bioanalytical method validation. We had established a new method that had been applied to the pharmacokinetic study of enasidenib in rats.

scholarly journals Targeted Quantitative Analysis ofStreptococcus pyogenesVirulence Factors by Multiple Reaction Monitoring

2008 ◽  
Vol 7 (8) ◽  
pp. 1489-1500 ◽  
Author(s):  
Vinzenz Lange ◽  
Johan A. Malmström ◽  
John Didion ◽  
Nichole L. King ◽  
Björn P. Johansson ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Multiple Reaction Monitoring ◽  
Reaction Monitoring

scholarly journals Development of UHPLC-MS/MS Method for Indirubin-3′-Oxime Derivative as a Novel FLT3 Inhibitor and Pharmacokinetic Study in Rats

Molecules ◽  
2020 ◽  
Vol 25 (9) ◽  
pp. 2039
Author(s):  
Na Yoon Kim ◽  
Yong-Chul Kim ◽  
Yoon Gyoon Kim
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Reaction Monitoring ◽  
Spectrometry Method ◽  
Limit Of Quantification ◽  
Flt3 Inhibitor ◽  
Pharmacokinetic Properties ◽  
Safety Guidelines ◽  
The U.S

This study aimed to develop and validate a sensitive liquid chromatography-coupled tandem mass spectrometry method for the quantification of LDD-2614, an indirubin derivative and novel FLT3 inhibitor, in rat plasma. In addition, the developed analytical method was applied to observe the pharmacokinetic properties of LDD-2614. Chromatographic separation was achieved on a Luna omega C18 column using a mixture of water and acetonitrile, both containing 0.1% formic acid. Quantitation was performed using positive electrospray ionization in a multiple reaction monitoring (MRM) mode. The MRM transitions were optimized as m/z 426.2→113.1 for LDD-2614 and m/z 390.2→113.1 for LDD-2633 (internal standard), and the lower limit of quantification (LLOQ) for LDD-2614 was determined as 0.1 ng/mL. Including the LLOQ, the nine-point calibration curve was linear with a correlation coefficient greater than 0.9991. Inter- and intraday accuracies (RE) ranged from −3.19% to 8.72%, and the precision was within 9.02%. All validation results (accuracy, precision, matrix effect, recovery, stability, and dilution integrity) met the acceptance criteria of the U.S. Food and Drug Administration and the Korea Ministry of Food and Drug Safety guidelines. The proposed method was validated and demonstrated to be suitable for the quantification of LDD-2614 for pharmacokinetics studies.

Alpha-Methylfentanyl and Beta-Hydroxyfentanyl LC–MS-MS Quantification in Rat Plasma after Long-Term Ethanol Exposure

2020 ◽  
Vol 44 (8) ◽  
pp. 896-904
Author(s):  
Lihong Lyu ◽  
Rui Chen ◽  
Lu Li ◽  
Hongbin Duan ◽  
Yao Chen ◽  
...  
Keyword(s):  
Illicit Drug ◽  
Matrix Effects ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Plasma Concentrations ◽  
Rat Plasma ◽  
Ethanol Exposure ◽  
Pharmacokinetic Parameters ◽  
Control Group ◽  
Science Field

Abstract Fentanyl and its analogues are highly abused drugs that dominate the illicit drug trade. alpha-Methylfentanyl (A-F) and beta-hydroxyfentanyl (B-F) are two fentanyl analogues that require the development of rapid detection technologies. The current study established and validated a rapid and high-sensitivity liquid chromatography–tandem mass spectrometry (LC–MS-MS) method to measure A-F and B-F concentrations in rat plasma following intravenous drug administration (20 μg/kg). Because fentanyl is primarily metabolized by the liver, we evaluated the concentrations of A-F and B-F in vivo in rats, in a control group and a group with liver damage induced by 55 days of oral ethanol gavage (6.5 g/kg, 22.5% v/v). Liquid–liquid extraction and LC–MS-MS operating in the positive ion multiple reaction monitoring mode were used. A C18 column was used, and the mobile phase consisted of 0.1% formic acid aqueous and acetonitrile. The limit of detection was 3 pg/mL (S/N &gt; 5) for A-F and B-F. The calibration curves were linear within the concentration range of 0.01–5 ng/mL (R2 = 0.9991) and 0.005–20 ng/mL (R2 = 0.9999) for A-F and B-F, respectively. Extraction recoveries were 91.3%–97.6% with RSD ≤ 11.2% and 90.5%–94.3% with RSD ≤ 10.5% for A-F and B-F, respectively. Plasma matrix effects were 80.61%–84.58% for A-F and 80.67%–81.33% for B-F with RSD ≤ 13.9%. The validated assay indicated no significant differences in pharmacokinetic parameters (AUC0-t, Cmax and T1/2) derived from the assessment of A-F and B-F plasma concentrations between control and ethanol-exposed rats. This assay, for which the LOD was 3 pg/mL for A-F and B-F may help the forensic science field to determine fentanyl analogue-related causes of death and identify illicit drug tampering.

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