Direct Sample Introduction for Large Bore Capillary Columns in Gas Chromatography

1963 ◽  
Vol 1 (5) ◽  
pp. 9-11 ◽  
Author(s):  
A. Zlatkis ◽  
J. Q. Walker
2000 ◽  
Vol 83 (3) ◽  
pp. 680-697 ◽  
Author(s):  
Steven J Lehotay

Abstract Direct sample introduction (DSI), or “dirty sample injection,” was investigated in the determination of 22 diverse pesticide residues in mixed apple, green bean, and carrot extracts by benchtop gas chromatography/tandem mass spectrometry (DSI/GC/MS–MS). The targeted pesticides, some of which were incurred in the samples, included chlorpyrifos, azinphos-methyl, parathion-methyl, diazinon, terbufos, p,p′-DDE, endosulfan sulfate, carbofuran, carbaryl, propargite, bifenthrin, dacthal, trifluralin, metalaxyl, pendimethalin, atrazine, piperonyl butoxide, diphenylamine, vinclozolin, chlorothalonil, quintozene, and tetrahydrophthalimide (the breakdown product of captan). The analytical DSI method entailed the following steps: (1) blend 30 g sample with 60 mL acetonitrile for 1 min in a centrifuge bottle; (2) add 6 g NaCl and blend 30 s; (3) centrifuge for 1–2 min; (4) add 5 mL upper layer to 1 g anhydrous MgSO4 in a vial; and (5) analyze 11 μL extract, using DSI/GC/MS–MS. Sample cleanup is not needed because GC/MS–MS is exceptionally selective for the targeted analytes, and nonvolatile coextracted matrix components do not contaminate the injector or the GC/MS–MS system. Average recoveries of the pesticides were 103 ± s7% with relative standard deviations of 14 ± 5% on average, and limits of detection were <2 ng/g for nearly all pesticides studied. The DSI/GC/MS–MS approach for targeted pesticides is quantitative, confirmatory, sensitive, selective, rugged, rapid, simple, and inexpensive.


2006 ◽  
Vol 89 (1) ◽  
pp. 40-45 ◽  
Author(s):  
Shikai Yan ◽  
Wenfeng Xin ◽  
Guoan Luo ◽  
Yiming Wang ◽  
Yiyu Cheng

Abstract A rapid, rugged, and inexpensive approach is described to develop chemical fingerprints of volatile and semivolatile fractions in herbal medicine. The method is based on the combination of direct sample introduction and gas chromatography (GC) analysis with mass spectrometry detection. In comparison with routine methods, the proposed approach provides the most informative fingerprint and does not demand time-consuming extraction, pretreatment, and cleanup procedures. The approach was applied to establish the GC fingerprint of gardenia fruit (Gardenia jasminoides Ellis), in which 39 components were identified. With the help of principal components analysis, the obtained fingerprint could reveal the variation in and within different herb samples as affected by season and developmental state (wild or cultivated). The results indicated that the proposed approach could serve as a rapid, simple, and effective technique for the quality control of herbal medicines.


Sign in / Sign up

Export Citation Format

Share Document