A rapid and sensitive liquid chromatography–tandem mass spectrometric assay for moexipril, an angiotensin‐converting enzyme inhibitor in human plasma

Karra, Vijaya Kumari; Mullangi, Ramesh; Pilli, Nageswara Rao; Inamadugu, Jaswanth Kumar; Ravi, Vasu Babu; Rao, J. V. L. N. Seshagiri

doi:10.1002/bmc.2731

Cited by 5 publications

(5 citation statements)

References 9 publications

(10 reference statements)

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“…Also, in 2012, Karra et al developed a method for determination of MOX by LC-Tandem mass spectrometry. But MOXT, which is the active metabolite was not determined [11].…”

Section: Moexipril (3s)-2-[(2s)-2-[[(1s)-1-(ethoxycarbonyl)-3-phenylpmentioning

confidence: 99%

“…It is reported that MOX was identified by HPLC [4][5][6], spectrophotometry [7,8], gas chromatography mass spectrometry [9], and liquid chromatography tandem mass spectrometry [10,11]. In 2006, Koti, J. et al developed a LC-MASS spectrometry method just to monitor the metabolism of MOX to MOXT [10].…”

Section: Moexipril (3s)-2-[(2s)-2-[[(1s)-1-(ethoxycarbonyl)-3-phenylpmentioning

confidence: 99%

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Liquid chromatography-electro spray ionization tandem mass spectrometry for simultaneous determination of Moexipril and its active metabolite Moexiprilat in human plasma

et al. 2014

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A selective, sensitive, and rapid liquid chromatography-electro spray ionization tandem mass spectrometry method has been developed and subsequently validated for the simultaneous determination of Moexipril (MOX), and its active metabolite Moexiprilat (MOXT) in spiked human plasma, using Benazepril (BENZ) as an internal standard (IS). Various modes were tried and the Multiple Reaction Monitoring (MRM) mode was found the most suitable one. The two analytes and Benazepril (IS) were extracted from human plasma by simple protein precipitation using acetonitrile as the precipitating solvent. The stationary phase used was a C18 Sunfire column while water and acetonitrile at 0.1% formic acid (30:70, v:v) was used as a mobile phase. The flow rate used was 0.8 mL/min. Food and Drug Administration guidelines were followed for the method validation. The linearity range was found to be 0.5-100 ng/mL for MOX and 5-200 ng/mL for MOXT and the correlation coefficient was more than 0.9980 for each analyte. Results for accuracy and precision showed satisfactory results. Also the method was compared with reported HPLC method and no significant difference was found.

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“…Also, in 2012, Karra et al developed a method for determination of MOX by LC-Tandem mass spectrometry. But MOXT, which is the active metabolite was not determined [11].…”

Section: Moexipril (3s)-2-[(2s)-2-[[(1s)-1-(ethoxycarbonyl)-3-phenylpmentioning

confidence: 99%

Section: Moexipril (3s)-2-[(2s)-2-[[(1s)-1-(ethoxycarbonyl)-3-phenylpmentioning

confidence: 99%

Liquid chromatography-electro spray ionization tandem mass spectrometry for simultaneous determination of Moexipril and its active metabolite Moexiprilat in human plasma

et al. 2014

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“…Moexiprilat, in human plasma [8]. Karraa et al developed a rapid and sensitive liquid chromatography-tandem mass spectrometric assay for MOX in human plasma [9]. As there are no reports available on the degradation behavior, identification and characterization of Degadaation Products (DPs) of MOX formed under various stress conditions, we have carried out a detailed study on stability indicating LC-MS/MS method for MOX.…”

Section: Biochemistry and Analytical Biochemistrymentioning

confidence: 99%

“…Finally we achieved a good resolution of peaks with acceptable shape with mobile phase consisting of 20 mM ammonium acetate buffer (A), pH adjusted to 6.0 using dilute formic acid and methanol (B) in a gradient elution program. The gradient program for mobile phase solvents was set as follows, (T min / %solution of B): 0-0 /30, 0-5 /65, [5][6][7][8][9][10][11][12][13][14][15] /65, 15-20 /30. The mobile phase flow rate of 1.0 ml/min, column temperature of 25°C and wavelength of 273 nm were found to be suitable for the chromatographic separation of MOX and its DPs.…”

Section: Optimization Of Lc-ms Conditionsmentioning

confidence: 99%

Identification and Characterization of Forced Degradation Products of Moexipril Using LC-ESI-MS/Q-TOF

Kb¹,

Nagaraju²,

Rajendra³

et al. 2018

Biochem Anal Biochem

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A forced degradation study on drug moexipril has been conducted to provide an insight into degradation products and degradation pathways as per International Conference on harmonization (ICH) Q1A (R2) guideline. Moexipril was subjected to stress conditions by hydrolysis (acidic, alkaline and neutral), oxidation, photolysis and thermal. The drug degraded in the stress conditions of hydrolysis, oxidation and photolysis but remained stable in conditions of thermal stress. A total of 5 degradation products were formed from the drug, which were separated by developed gradient liquid chromatographic method on a C-18 column (4.6 × 150 mm, 5 μm) by gradient elution technique using ammonium acetate buffer and methanol at mobile phase flow rate of 1.0 mL/min at 25°C. The degradation products were identified and structurally elucidated by using liquid chromatography with quadrupole time of flight electrospray ionization tandem mass spectrometer combined accurate mass measurements. The most probable structures for the observed degradation products were assigned by comparing the product ions of all the protonated degradation products with the product ions of protonated moexipril.

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“…Karra et al () have reported LC–MS method for quantitative determination of moexipril in human plasma. An HPLC method for the quantitative determination of moexipril in pharmaceutical dosage forms was developed and applied to the assay of moexipril in tablet and bulk form (Elshanawane, Mostafa, & Elgawish, ).…”

Section: Introductionmentioning

confidence: 99%

Structural identification of degradants of moexipril by LC–MS/MS

Challa¹,

Ramakrishna

Rao³

2017

Biomedical Chromatography

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A gradient LC-MS method was developed for the identification and characterization of degradants of moexipril using liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Moexipril was subjected to hydrolysis (acid, base and neutral), oxidation, photolytic and thermal degradation conditions as mentioned in ICH guidelines Q1A (R2). The drug degraded under hydrolysis, oxidation and photolytic conditions, but it was stable under thermal conditions. In total, five degradants were formed and separated on an Agilent XDB C-18 column (4.6 × 150 mm, 5 μm) in a gradient elution method. Four degradants (D1, D2, D4 and D5) under acidic conditions, three degradants (D2, D3 and D4) under basic conditions and three degradants (D1, D4 and D5) under neutral and oxidative stress conditions were formed. In addition, two degradants (D4 and D5) were formed under photolytic stress conditions. To elucidate the structures of degradants, fragmentation of moexipril and its degradants was studied using LC-MS/MS experiments and accurate mass measurements (HRMS) data. The fragment ions in the product ion tandem mass spectra of all the degradants were compared with those of moexipril and assigned the probable structures for the degradants.

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A rapid and sensitive liquid chromatography–tandem mass spectrometric assay for moexipril, an angiotensin‐converting enzyme inhibitor in human plasma

Cited by 5 publications

References 9 publications

Liquid chromatography-electro spray ionization tandem mass spectrometry for simultaneous determination of Moexipril and its active metabolite Moexiprilat in human plasma

Liquid chromatography-electro spray ionization tandem mass spectrometry for simultaneous determination of Moexipril and its active metabolite Moexiprilat in human plasma

Identification and Characterization of Forced Degradation Products of Moexipril Using LC-ESI-MS/Q-TOF

Structural identification of degradants of moexipril by LC–MS/MS

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