scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

scholarly journals Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Alverine and its Metabolite, Monohydroxy Alverine, in Human Plasma: Application to a Pharmacokinetic Study

2011 ◽  
Vol 8 (1) ◽  
pp. 201-211 ◽  
Author(s):  
Rahul C. Gavhane ◽  
Ketan K. Nerurkar ◽  
Ashok M. Kalamkar ◽  
Mitesh R. Patil ◽  
Satish G. Pingale ◽  
...  
Keyword(s):  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Solid Phase ◽  
Internal Standard ◽  
Selected Reaction Monitoring ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Assay Precision ◽  
Male Subjects

A rapid and sensitive LC-MS-MS method for the determination of alverine (ALV) and its major metabolite, monohydroxy alverine (MHA), in human plasma using imipramine as an internal standard was developed and validated. The analytes were extracted from 0.5 mL aliquots of human plasma by solid phase extraction, using oasis cartridge. Chromatographic separation was carried on Thermo Gold C18 column (50 × 4.6 mm, 5 μ) at 30 °C, with isocratic mobile phase, a flow rate of 0.4 mL/min and a total run time of 3.5 min. Detection and quantification were performed using a mass spectrometer in the selected reaction-monitoring mode with positive electrospray ionization atm/z282.3 → 91.11 for alverine,m/z298.3 → 106.9 for mono-hydroxy-alverine, andm/z281.0 → 86.0 for internal standard (IS) respectively. This assay was linear over a concentration range of 0.060-10 ng/mL with a lower limit of quantification of 0.060 ng/mL for both alverine and monohydroxy alverine. The coefficient of variation for the assay precision were <9.18% and <8.44%, the accuracy were >104.66% and >100.38% for alverine and monohydroxy alverine respectively. This method was successfully applied to a pharmacokinetic study after oral administration of alverine citrate 60 mg capsule in healthy male subjects.

On-Line Solid Phase Extraction Using the Prospekt-2 Coupled with a Liquid Chromatography/Tandem Mass Spectrometer for the Determination of Dextromethorphan, Dextrorphan and Guaifenesin in Human Plasma

2005 ◽  
Vol 11 (2) ◽  
pp. 199-208 ◽  
Author(s):  
Debbie L. Kuhlenbeck ◽  
Thomas H. Eichhold ◽  
Steven H. Hoke ◽  
Timothy R. Baker ◽  
Robert Mensen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Human Plasma ◽  
Solid Phase ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
On Line

An on-line liquid chromatography/tandem mass spectrometry (LC-MS/MS) procedure, using the Prospekt-2 system, was developed and used for the determination of the levels of the active ingredients of cough/cold medications in human plasma matrix. The experimental configuration allows direct plasma injection by performing on-line solid phase extraction (SPE) on small cartridge columns prior to elution of the analyte(s) onto the analytical column and subsequent MS/MS detection. The quantitative analysis of three analytes with differing polarities, dextromethorphan (DEX), dextrorphan (DET) and guaifenesin (GG) in human plasma presented a significant challenge. Using stable-isotope-labeled internal standards for each analyte, the Prospekt-2 on-line methodology was evaluated for sensitivity, suppression, accuracy, precision, linearity, analyst time, analysis time, cost, carryover and ease of use. The lower limit of quantitation for the on-line SPE procedure for DEX, DET and GG was 0.05, 0.05 and 5.0 ng mL−1, respectively, using a 0.1 mL sample volume. The linear range for DEX and DET was 0.05–50 ng mL−1 and was 5–5,000 ng mL−1 for GG. Accuracy and precision data for five different levels of QC samples were collected over three separate days. Accuracy ranged from 90% to 112% for all three analytes, while the precision, as measured by the %RSD, ranged from 1.5% to 16.0%.

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