scholarly journals A RAPID, SENSITIVE AND VALIDATED ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY AND TANDEM MASS SPECTROMETRY METHOD FOR DETERMINATION OF PAROMOMYCIN IN MICE PLASMA: APPLICATION TO PHARMACOKINETIC STUDY

2017 ◽  
Vol 9 (5) ◽  
pp. 86 ◽  
Author(s):  
M. Jakir S. K. Pinjari ◽  
Rahul S. Somani ◽  
Ritu M. Gilhotra
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Ultra Performance Liquid Chromatography ◽  
Precipitation Method ◽  
Plasma Samples ◽  
Spectrometry Method ◽  
Multiple Reactions ◽  
The Mean ◽  
Precision And Accuracy

Objective: To develop and validate simple, sensitive, accurate and selective UPLC-MS/MS method for quantification of paromomycin (PARO) in mice plasma.Methods: Precipitation method was used for the extraction of plasma samples, an aliquot of 25 µl plasma samples was extracted using 10% perchloric acid in water. Chromatographic separation was performed using waters acquity ultra-performance liquid chromatography (UPLC) columns, BEH HILIC (50 mm× 2.1 mm, 1.7 µm) by a gradient mixture of acetonitrile and water (both containing 0.005% v/v trifluro acetic acid) as a mobile phase at the flow rate of 0.2 ml/min. The analyte was protonated in the positive electrospray ionization (ESI) interface and detected in multiple reactions monitoring (MRM) modes using the transition m/z 308.60-455.30.Results: The method had a short chromatographic run time of 3 min. Calibration curves were linear over wide ranges of 50.51-5019.22 ng/ml. The between and within-batch precision and accuracy of the method was determined by using 4 quality control samples, the highest % CV observed was 11.06. The mean recovery values are 78.17, 101.17 and 92.58 at low, medium and high-quality control levels; respectively.Conclusion: It was concluded that the developed and validated UPLC-MS/MS method was rapid, sensitive, accurate, precise, linear, and specific. Therefore, this method can be used for quantification of PARO in mice plasma with various advantages over the reported methods.

ENZYMATISCH-FLUOROMETRISCHE BESTIMMUNG DER CORTISOLBINDUNGSKAPAZITÄT DES PLASMA

1967 ◽  
Vol 56 (1) ◽  
pp. 99-106 ◽  
Author(s):  
K. Leybold ◽  
J. Rieper ◽  
L. Weissbecker
Keyword(s):  
Binding Capacity ◽  
Liver Microsomes ◽  
Mean Value ◽  
Female Rats ◽  
Plasma Samples ◽  
Simple Method ◽  
Adult Men ◽  
The Mean ◽  
Precision And Accuracy

ABSTRACT A simple method for the determination of cortisol-binding capacity is described. For saturation of the cortisol-binding proteins, plasma samples are incubated with an excess of cortisol. In the next step NADPH and liver microsomes of female rats are added. The microsomal Δ4-3-ketosteroid hydrogenase only reduces non protein-bound cortisol to tetrahydrocortisol-5α. Then the steroids are extracted by dichloromethane, and after some purification steps analyzed by fluorometry. Tetrahydrocortisol gives practically no fluorescence. The cortisol determined by this method corresponds to protein-bound cortisol and indicates the extent of cortisolbinding capacity. Precision and accuracy of the method were found to be good. The values of cortisol-binding capacity obtained by our method are compared with the results of other authors. The mean value of adult men was 25.5 ± 3.4 μg/100 ml, that of pregnant women, mens IX-X, 42.3 ± 4.2 μg/100 ml.

scholarly journals A RAPID, SENSITIVE AND VALIDATED ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY AND TANDEM MASS SPECTROMETRY METHOD FOR DETERMINATION OF RIFAMPICIN IN RAT PLASMA: APPLICATION TO PHARMACOKINETIC STUDY

2017 ◽  
Vol 9 (2) ◽  
pp. 222
Author(s):  
Aslam Burhan ◽  
Bhavin Vyas
Keyword(s):  
Mass Spectrometry ◽  
Quality Control ◽  
Liquid Chromatography ◽  
Drug Interaction ◽  
Tandem Mass Spectrometry ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Plasma Samples ◽  
Interaction Studies

<p><strong>Objective: </strong>To develop and validate simple, sensitive and selective ultra-performance liquid chromatography and tandem mass spectrometry (UPLC-MS/MS) method for quantification of rifampicin (RIF) in rat plasma and its application to pharmacokinetics study.</p><p><strong>Methods: </strong>Precipitation method was used for the extraction of plasma samples, an aliquot of 25 µl plasma samples was extracted using acetonitrile precipitation technique. Chromatographic separation was performed usingWaters Acquity<sup>TM</sup>UPLC columns, BEH C18 (50 mm× 2.1 mm, 1.7 µm) by a gradient mixture of acetonitrile and water (both containing 0.1 % formic acid) as a mobile phase at the flow rate of 0.7 ml/min.The analyte was protonated in the positive ESI (electrospray ionization interface) and detected in MRM (multiple reactions monitoring) modes using the transition m/z 308.60-455.30.</p><p><strong>Results: </strong>The method had a short chromatography run time of 1.8 min with improved sensitivity over existing methods. Calibration curves been linear over the wide range of 1.97-5047.00 ng/ml. The between and within-batch precision and accuracy of the method was determined by using 4 quality control samples; the highest %CV observed was10.11. The mean recovery values are 74.26, 82.77 and 101.73 at low, medium and high-quality control levels; respectively.</p><p><strong>Conclusion: </strong>It was concluded that the developed and validated UPLC-MS/MS method was sensitive,specific, precise, linear, and rapid. Therefore, the method can be used for quantification of RIFin rat plasma with various advantages over the reported methods. RIF is widely recommended by US-FDAguidance for industry on drug interaction studies and the developed method can be used to explore drug interaction studies in drug discovery and development.</p>

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