Guanidinated protein internal standard for immunoaffinity-liquid chromatography/tandem mass spectrometry quantitation of protein therapeutics

Background: Dehydroepiandrosterone sulphate (DHEAS) is a steroid that is increasingly being recognized as a potential drug of abuse in many countries. This is due to its reputation as a hormone that may be able to retard the ageing process. The measurement of DHEAS is useful in the diagnosis of medical conditions such as congenital adrenal hyperplasia and polycystic ovary syndrome. Thus, a liquid chromatography-tandem mass spectrometry method has been developed to determine DHEAS concentrations in human serum. Method: The chromatography was performed using a WatersTM 2795 Alliance HT LC system coupled to a Mercury Fusion-RP column fitted with a SecurityGuardTM column. Results: DHEAS and the internal standard, deuterated DHEAS, both had a retention time of 1.5 min. The transition determined by the Micromass QuattroTM tandem mass spectrometer for DHEAS was m/z 367.3>96.7 and for the internal standard m/z 369.3>96.6. The method was linear up to 20 µmol/L; the lower limit of detection and the lower limit of quantitation were both 1 µmol/L. The intra- and interassay imprecision were <11% over a concentration range of 1-18 µmol/L for the in-house quality control and <12% for the intra- and interassay imprecision for the Bio-Rad Lyphocheck QC. Conclusion: The measurement of DHEAS by liquid chromatography-tandem mass spectrometry is robust and has a simple sample preparation procedure with a rapid cycle time of only 4 min.

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Simultaneous quantification of losartan and active metabolite in human plasma by liquid chromatography–tandem mass spectrometry using irbesartan as internal standard

Journal of Pharmaceutical and Biomedical Analysis ◽

10.1016/j.jpba.2009.01.007 ◽

2009 ◽

Vol 49 (3) ◽

pp. 862-867 ◽

Cited By ~ 22

Author(s):

Budi Prasaja ◽

Lucy Sasongko ◽

Yahdiana Harahap ◽

Hardiyanti ◽

Windy Lusthom ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Human Plasma ◽

Active Metabolite ◽

Internal Standard ◽

Tandem Mass ◽

Simultaneous Quantification ◽

Chromatography Tandem Mass Spectrometry ◽

Liquid Chromatography Tandem Mass

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Liquid Chromatography-Tandem Mass Spectrometry of Desoxo-Narchinol a and Its Pharmacokinetics and Oral Bioavailability in Rats and Mice

Molecules ◽

10.3390/molecules24112037 ◽

2019 ◽

Vol 24 (11) ◽

pp. 2037 ◽

Cited By ~ 2

Author(s):

Subindra Kazi Thapa ◽

Mahesh Upadhyay ◽

Tae Hwan Kim ◽

Soyoung Shin ◽

Sung-Joo Park ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Oral Bioavailability ◽

Internal Standard ◽

Rat Plasma ◽

Tandem Mass ◽

Mouse Plasma ◽

Chromatography Tandem Mass Spectrometry ◽

Liquid Chromatography Tandem Mass

Desoxo-narchinol A is one of the major active constituents from Nardostachys jatamansi, which has been reported to possess various pharmacological activities, including anti-inflammatory, antioxidant, and anticonvulsant activity. A simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of desoxo-narchinol A in two different biological matrices, i.e., rat plasma and mouse plasma, using sildenafil as an internal standard (IS). The method involved simple protein precipitation with acetonitrile and the analyte was separated by gradient elution using 100% acetonitrile and 0.1% formic acid in water as a mobile phase. The MS detection was performed with a turbo electrospray in positive ion mode. The lower limit of quantification was 10 ng/mL in both rat and mouse plasma. Intra- and inter-day accuracies were in the ranges of 97.23–104.54% in the rat plasma and 95.90–110.11% in the mouse plasma. The precisions were within 8.65% and 6.46% in the rat and mouse plasma, respectively. The method was applied to examine the pharmacokinetics of desoxo-narchinol A, and the oral bioavailability of desoxo-narchinol A was 18.1% in rats and 28.4% in mice. The present results may be useful for further preclinical and clinical studies of desoxo-narchinol A.

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A Hydrophilic Interaction Liquid Chromatography–Tandem Mass Spectrometry Quantitative Method for Determination of Baricitinib in Plasma, and Its Application in a Pharmacokinetic Study in Rats

Molecules ◽

10.3390/molecules25071600 ◽

2020 ◽

Vol 25 (7) ◽

pp. 1600 ◽

Cited By ~ 1

Author(s):

Essam Ezzeldin ◽

Muzaffar Iqbal ◽

Yousif A. Asiri ◽

Azza A Ali ◽

Prawez Alam ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Multiple Reaction Monitoring ◽

Internal Standard ◽

Janus Kinase ◽

Pharmacokinetic Studies ◽

Tandem Mass ◽

Chromatography Tandem Mass Spectrometry ◽

Liquid Chromatography Tandem Mass

Baricitinib, is a selective and reversible Janus kinase inhibitor, is commonly used to treat adult patients with moderately to severely active rheumatoid arthritis (RA). A fast, reproducible and sensitive method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantification of baricitinib in rat plasma has been developed. Irbersartan was used as the internal standard (IS). Baracitinib and IS were extracted from plasma by liquid–liquid extraction using a mixture of n-hexane and dichloromethane (1:1) as extracting agent. Chromatographic separation was performed using Acquity UPLC HILIC BEH 1.7 µm 2.1 × 50 mm column with the mobile phase consisting of 0.1% formic acid in acetonitrile and 20 mM ammonium acetate (pH 3) (97:3). The electrospray ionization in the positive-mode was used for sample ionization in the multiple reaction monitoring mode. Baricitinib and the IS were quantified using precursor-to-production transitions of m/z 372.15 > 251.24 and 429.69 > 207.35 for baricitinib and IS, respectively. The method was validated according to the recent FDA and EMA guidelines for bioanalytical method validation. The lower limit of quantification was 0.2 ng/mL, whereas the intra-day and inter-day accuracies of quality control (QCs) samples were ranged between 85.31% to 89.97% and 87.50% to 88.33%, respectively. Linearity, recovery, precision, and stability parameters were found to be within the acceptable range. The method was applied successfully applied in pilot pharmacokinetic studies.

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Development and validation of bioanalytical liquid chromatography–tandem mass spectrometry method for the estimation of pentoxifylline in human plasma: Application for a comparative pharmacokinetic study

European Journal of Mass Spectrometry ◽

10.1177/1469066718817929 ◽

2018 ◽

Vol 25 (4) ◽

pp. 372-380 ◽

Cited By ~ 1

Author(s):

Sireesha Dodda ◽

Ajitha Makula ◽

Srinivasa R Polagani ◽

Raj N Kandhagatla

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Human Plasma ◽

Pharmacokinetic Study ◽

Internal Standard ◽

Tandem Mass ◽

Comparative Pharmacokinetic ◽

Chromatography Tandem Mass Spectrometry ◽

Liquid Chromatography Tandem Mass

A method for bioanalysis of pentoxifylline in human plasma was developed using liquid chromatography–tandem mass spectrometry, which is simple, specific, and sensitive. Pentoxifylline D5 was used as the internal standard. Employing only 100 µl of human plasma, processing was done with solid-phase extraction technique. The analyte and the internal standard were separated from endogenous components on Ace phenyl column using a mixture of 5 mM ammonium acetate buffer and high performance liquid chromatography grade acetonitrile (60:40, v/v) as mobile phase at a flow rate of 1 ml/min. The linearity of the method was in the range of 3–1200 ng/ml with r2 > 0.99. Positive ion MRM mode was used for the detection of the analyte and the internal standard. The method was validated as per the US Food and Drug Administration guidelines and the results were within the acceptance limits. The proposed method was applied for comparative pharmacokinetic study of pentoxifylline after oral administration of 400 and 600 mg tablets to South Indian male subjects under fed conditions.

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