Determination of Aspirin and Salicylic Acid in Human Plasma by Column-Switching Liquid Chromatography Using On-Line Solid-Phase Extraction

1998 ◽  
Vol 70 (2) ◽  
pp. 409-414 ◽  
Author(s):  
Gillian P. McMahon ◽  
Mary T. Kelly
Keyword(s):  
Salicylic Acid ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Human Plasma ◽  
Solid Phase ◽  
Column Switching ◽  
Phase Extraction ◽  
On Line

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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