Purge-and-Trap Analysis Using Fused Silica Capillary Column GC/MS

1983 ◽  
Vol 21 (3) ◽  
pp. 111-118 ◽  
Author(s):  
F. A. Dreisch ◽  
T. O. Munson
1986 ◽  
Vol 32 (3) ◽  
pp. 503-505 ◽  
Author(s):  
C W Jones

Abstract This mass-spectrometric method for assaying tocainide in serum is specific, reproducible, and sensitive, and sample preparation is rapid. The drug is isolated from serum by liquid-solid extraction on a Baker C18 disposable column. Underivatized drug is separated by elution on a 0.20 mm X 25 m fused-silica capillary column coated with 5% phenylmethylsilicone, then quantified by mass-selective detection (selected ion monitoring). Sample size is 1 mL of serum, but smaller volumes may be used. Mean analytical recovery of the drug from the disposable columns is 75%. Commonly used antiarrhythmics, sedatives, or hypnotics do not interfere. The run-to-run CV at 3.7 mg/L is 4.0%, 3.0% at 10.5 mg/L.


1981 ◽  
Vol 4 (8) ◽  
pp. 366-384 ◽  
Author(s):  
A. D. Sauter ◽  
L. D. Betowski ◽  
T. R. Smith ◽  
V. A. Strickler ◽  
R. G. Beimer ◽  
...  

1992 ◽  
Vol 75 (4) ◽  
pp. 729-733 ◽  
Author(s):  
Michael W Ogden

Abstract Alternative gas chromatographic (GC) conditions were collaboratively studied for equivalency with conditions specified in the official AOAC method 990.01 for nicotine in environmental tobacco smoke (ETS). Test conditions under evaluation were the use of a 30 m x 0.32 mm id fused silica capillary column with split injection as compared to the method-specified 30 m x 0.53 mm id fused silica capillary column with direct or on-column injection. The 6 samples analyzed in duplicate by 7 laboratories included 3 spiked samples (concentration ranging from 0.18 to 1.8 µ.g nicotine per sample) and 3 ETS samples (concentration in air ranging from 4 to 36 µg nicotine/cu m). Four laboratories used the AOAC approved GC conditions and 3 used the test conditions. Data analysis detected no difference in results (P= 0.72) obtained using either the 0.32 mm or 0.53 mm id column (and associated conditions). Average repeatability (RSDr) and reproducibility (RSDR) relative standard deviations for the 0.53 mm id column were 5.2 and 8.3%, respectively, for spiked nicotine samples, and 5.3 and 8.5%, respectively, for ETS samples. Average repeatability (RSDr) and reproducibility (RSDR) relative standard deviations for the 0.32 mm id column were 4.1 and 4.7%, respectively, for spiked nicotine samples, and 3.5 and 6.3%, respectively, for ETS samples. The method incorporating the use of the 0.32 mm id column and associated conditions is recommended for adoption as official first action.


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