scholarly journals Screening Procedure for Detection of Non-Steroidal Anti-inflammatory Drugs and their Metabolites in Urine as Part of a Systematic Toxicological Analysis Procedure for Acidic Drugs and Poisons by Gas Chromatography- Mass Spectrometry after Extractive Methylation*

2001 ◽  
Vol 25 (4) ◽  
pp. 237-244 ◽  
Author(s):  
Hans H. Maurer ◽  
François X. Tauvel ◽  
Thomas Kraemer
2011 ◽  
Vol 23 (4) ◽  
pp. 205-210 ◽  
Author(s):  
Maria Concetta Rotolo ◽  
Manuela Pellegrini ◽  
Devasish Bose ◽  
Emilia Marchei ◽  
Abhilasha Durgbanshi ◽  
...  

1991 ◽  
Vol 37 (11) ◽  
pp. 1975-1978 ◽  
Author(s):  
K E Brooks ◽  
N B Smith

Abstract We describe a method for efficiently extracting basic, neutral, and weakly acidic drugs from plasma for toxicological analysis by gas chromatography-mass spectrometry (GC/MS). The 2-mL plasma sample is diluted with an equal volume of saturated NaCl containing triethylamine, 10 mmol/L, and then extracted twice with 4 mL of an equivolume solution of dichloromethane/acetone. The organic (top) phases are combined, then mixed with 1 mL of water, 200 mg of NaHCO3, and 100 microliters of acetic anhydride. This mixture is then heated at 75 degrees C until the solvents have boiled off and aqueous acetylation is complete (less than 30 min). After addition of 1 mL of water and 2 g of NaCl, the sample is extracted twice with 2 mL of dichloromethane/acetone (2/1 by vol). The combined extracts are dried and then subjected to thin-layer chromatography on a blank Toxi-Lab Toxi-A chromatogram with 1-chlorobutane as the developing solvent (about 6 min). After the lipids have migrated with the mobile phase, the drugs are eluted from the origin with acetone/triethylamine (29/1 by vol), evaporated, and reconstituted in injection solvent. With this procedure drugs are recovered relatively quickly (less than 2 h) and the GC/MS total ion chromatograms are very clean. Studies with 13 basic, neutral, and weakly acidic drugs showed that all except theophylline were extracted with recoveries of at least 75%.


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