Ultra-performance liquid chromatography–tandem mass spectrometric determination of ramipril in human plasma

Purpose: To develop a sensitive and accurate ultra-performance liquid chromatography–tandem mass spectrometric (UPLC-MS) method for quantification of ramipril in human plasma.Methods: Ramipril was extracted from biological fluid using equal volumes of n-hexane and propanol (1:1, v/v), and then chromatographed in a suitable C18 column with methanol: 0.1 % HCOOH (4: 1, v/v) as mobile phase. Atorvastatin was used as an internal standard for the chromatographic separation and quantification. The method was validated according to the United States Food and Drug Administration guidelines for standard indices.Results: Ramipril was determined in the concentration range 0.05 and 1000 ng/mL the validation procedure exhibited a correlation coefficient of 0.9979 + 0.002 (p = 0.05). The studied drug was quantified with lower ceiling of 0.05 ng/mL, and showed an accuracy of 105.00 %.Conclusion: A sensitive UPLC-MS analytical method has been successfully developed for the quantification of ramipril in human plasma. This method can be applied efficiently for the quantification of ramipril in bioavailability and pharmacokinetic studies. Keywords: Liquid chromatography–tandem mass, Ramipril, Stability, Biological fluids, Plasma

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Validation of a Liquid Chromatography-Tandem Mass Spectrometric Assay for Quantitative Analysis of Lenvatinib in Human Plasma

International Journal of Analytical Chemistry ◽

10.1155/2017/2341876 ◽

2017 ◽

Vol 2017 ◽

pp. 1-6 ◽

Cited By ~ 3

Author(s):

Tomoko Ogawa-Morita ◽

Yoshiyuki Sano ◽

Tomoka Okano ◽

Hirofumi Fujii ◽

Makoto Tahara ◽

...

Keyword(s):

Liquid Chromatography ◽

Quantitative Analysis ◽

Human Plasma ◽

Matrix Effect ◽

Antineoplastic Agent ◽

Mass Spectrometric ◽

Pharmacokinetic Studies ◽

Tandem Mass ◽

Liquid Chromatography Tandem Mass ◽

Tandem Mass Spectrometric

Toward conducting clinical pharmacokinetic studies of an antineoplastic agent, lenvatinib, we developed a liquid chromatography-tandem mass spectrometric assay for its quantitative analysis in human plasma. Analyte (lenvatinib) and internal standard (IS, propranolol) in the plasma were extracted by using acetonitrile and chromatographically separated by using a XTerra MS C18 column with 0.2 mL/min flow and mobile phase starting with 0.1% formic acid in water, followed by increasing percentage of acetonitrile. Detection was performed by using combined reversed-phase liquid chromatography-tandem mass spectrometry (LC/MS-MS) with positive ion electrospray ionization. MS-MS ion transitions used were 427.602>371.000 for lenvatinib and 260.064>116.005 for IS. This study was validated for accuracy, precision, linearity, range, selectivity, lower limit of quantification, recovery, and matrix effect according to the Guideline on Bioanalytical Method Validation in Pharmaceutical Development in Japan. Calibration curve was plotted by using lenvatinib concentrations ranging within 9.6–200 ng/mL, and correlation coefficients (r2) were in excess of 0.997. Intra- and interday accuracy ranged within 95.8–108.3% with mean recoveries of 66.8% for lenvatinib, and precision was <6.7% at all quality control concentration levels. Matrix effect analysis showed extraction efficiency of 15.7% for lenvatinib. Collectively, these findings demonstrate the feasibility of this method to evaluate kinetic disposition of lenvatinib.

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Ultra-performance liquid chromatography-tandem mass spectrometric method for quantitation of the recently Food and Drug Administration approved combination of vaborbactam and meropenem in human plasma

Royal Society Open Science ◽

10.1098/rsos.200635 ◽

2020 ◽

Vol 7 (7) ◽

pp. 200635

Author(s):

Ahmed K. Kammoun ◽

Alaa Khedr ◽

Ahdab N. Khayyat ◽

Maha A. Hegazy

Keyword(s):

Liquid Chromatography ◽

Human Plasma ◽

Drug Administration ◽

Ultra Performance Liquid Chromatography ◽

Mass Spectrometric ◽

Spectrometric Method ◽

Tandem Mass ◽

Mass Spectrometric Method ◽

Liquid Chromatography Tandem Mass ◽

Tandem Mass Spectrometric

A parenteral medical combination containing vaborbactam and meropenem is used mainly to treat complicated urinary tract infections. A novel ultra-performance liquid chromatography tandem mass spectrometric method was developed for the sensitive determination of both compounds in human plasma. Sample preparation was performed by precipitation technique. The chromatographic separation was accomplished using the Acquity C18-BEH column, 0.01 M ammonium formate: acetonitrile (47 : 53, v/v) as a mobile phase with a flow rate of 0.2 ml min −1 . Analytes were monitored by applying multiple reaction monitoring. The bioanalytical validation criteria were conducted following the Food and Drug Administration recommendations. The method was linear within range 0.5 to 50 µg ml −1 , for both drugs. The intra-day and inter-day precision, as coefficient variation (% CV) and the accuracy, as % bias did not exceed 15% for both drugs. The percentage recovery of targeted analytes was not less than 77%, calculated at three quality control levels. The proposed method showed a suitable lower level of quantification value of 0.50 µg ml −1 for both analytes, which is far lower than the expected C max , which permits the use of this method for pharmacokinetic studies. The proposed method proved to be useful for the evaluation of this combination in both human plasma and pharmaceutical formulation.

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A Validated High-Performance Liquid Chromatography-Tandem Mass Spectrometric (Lc-Ms/Ms) Method for Simultaneous Determination of R(+)-Ketorolac and S(−)-Ketorolac in Human Plasma and Its Application to a Bioequivalence Study

Chromatography Research International ◽

10.4061/2011/214793 ◽

2011 ◽

Vol 2011 ◽

pp. 1-11 ◽

Cited By ~ 3

Author(s):

Sabyasachi Patri ◽

Anil K. Patni ◽

Sunil S. Iyer ◽

Arshad H. Khuroo ◽

Tausif Monif ◽

...

Keyword(s):

Liquid Chromatography ◽

Human Plasma ◽

Solid Phase ◽

Multiple Reaction Monitoring ◽

Internal Standard ◽

Bioequivalence Study ◽

Mass Spectrometric ◽

Tandem Mass ◽

Liquid Chromatography Tandem Mass ◽

Tandem Mass Spectrometric

We report a selective, accurate, and reproducible liquid chromatography-tandem mass spectrometric (LC-MS/MS) method that employs solid phase extraction for quantification of ketorolac enantiomers in human plasma. Resolution of R(+)-ketorolac and S(−)-ketorolac was achieved using a Chiral-AGP column and a mobile phase of ammonium formate buffer (10 mM, pH ):acetonitrile (85 : 15, v/v and 70 : 30, v/v) in a gradient time program. S(+)-etodolac was used as the internal standard (IS). Quantification was achieved using a positive electrospray ionization (ESI+) interface under multiple reaction monitoring (MRM) condition. The method was validated over the concentration range of 9.36–1198.69 ng/ml for R(+)-ketorolac and 6.07–776.74 ng/ml for S(−)-ketorolac. Matrix effect was found negligible and the method showed good performances in terms of accuracy (89.6–102.7%) and precision (1.7–6.7%) for both enantiomers. Extraction recoveries of R(+)-ketorolac, S(−)-ketorolac, and S(+)-etodolac were 82.04, 70.94, and 93.90%, respectively. Results of all stability exercises in human plasma were within acceptable limits. The method was successfully applied to a single dose cross over bioequivalence study in healthy human male volunteers. Incurred Sample Reanalysis (ISR) was performed by randomly selecting 10% of total subject samples of the study using Statistical Analysis Software (SAS). Values of 91.1% for R (+)-ketorolac and 83.5% for S(−)-ketorolac indicated good acceptance for ISR.

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Development and validation of a liquid chromatography-tandem mass spectrometric method for the determination of lenalidomide in human plasma and its application on bioequivalence studies

Journal of Analytical Science & Technology ◽

10.1186/s40543-019-0195-z ◽

2019 ◽

Vol 10 (1) ◽

Author(s):

R. Gopinath ◽

S. T. Narenderan ◽

M. Kumar ◽

B. Babu

Keyword(s):

Liquid Chromatography ◽

Human Plasma ◽

Internal Standard ◽

Spectrometric Method ◽

Tandem Mass ◽

Mass Spectrometric Method ◽

Mass Detection ◽

Triple Quadrupole Mass Spectrometer ◽

Liquid Chromatography Tandem Mass ◽

Tandem Mass Spectrometric

AbstractA simple, sensitive, and specific liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) method was developed and validated for the quantification of lenalidomide in human plasma. The separation was carried out on a symmetry, C18, 5-μm (50 × 4.6 mm) column as stationary phase and with an isocratic mobile phase of 0.1% formic acid in water-methanol in the ratio of (15:85, v/v) at a flow rate of 0.5 mL/min. Protonated ions formed by electrospray ionization in the positive mode were used to detect analyte and fluconazole (internal standard). The mass detection was made by monitoring the fragmentation of m/z 260.1/148.8 for lenalidomide and m/z 307.1/238.0 for internal standard on a triple quadrupole mass spectrometer. The developed method was validated over the concentration range of 10–1000 ng/mL for lenalidomide in human plasma with a correlation coefficient (r2) was 0.9930. The accuracy and precision values obtained from six different sets of quality control samples analyzed on separate occasions ranged from 99.41 to 106.97% and 2.88 to 4.22%, respectively. Mean extraction recoveries were 98.06% and 88.78% for the analyte and IS, respectively. The developed method was successfully applied for analyzing lenalidomide in human plasma samples.

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