Flame ionization detector supercritical fluid chromatography

ECD = electron capture detector FID = flame ionization detector GC = gas chromatography HRGC = high resolution gas chromatography LC-APCI-MS = liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry LSE = liquid-solid extraction MS = mass spectrometry PVC = polyvinyl chloride SFE = supercritical fluid extraction... 

One example of normal-phase liquid chromatography coupled to gas chromatography is the determination of alkylated, oxygenated and nitrated polycyclic aromatic compounds (PACs) in urban air particulate extracts (97). Since such extracts are very complex, LC-GC is the best possible separation technique. A quartz microfibre filter retains the particulate material and supercritical fluid extraction (SPE) with CO2 and a toluene modifier extracts the organic components from the dust particles. The final extract is then dissolved in -hexane and analysed by NPLC. The transfer at 100 p.1 min of different fractions to the GC system by an on-column interface enabled many PACs to be detected by an ion-trap detector. A flame ionization detector (PID) and a 350 p.1 loop interface was used to quantify the identified compounds. The experimental conditions employed are shown in Table 13.2. 

The amount detected by this system (0.3pg on column) was below the level which could have been determined using a flame ionization detector. Initial indications show that the photoionization detector may be a very useful detector for people who wish to get to lower levels on the supercritical fluid chromatography and cannot concentrate their sample. 

Hadj-Mahammed, M., Badjah-Hadj-Ahmed, Y., and Meklati, B.Y., Behavior of pol5nnethoxy-lated and polyhydroxylated flavones by carbon dioxide supercritical fluid chromatography with flame ionization and Fourier transform infrared detectors, Phytochem. Anal, 4, 275, 1993. 

Artemisinin 9a has been extracted from Artemisia annua L. by supercritical fluid extraction and analyzed by supercritical fluid chromatography (SFC) using a capillary column coupled with a flame ionization detector <1997JCFI(A)353>. The SFC method has also been used for the determination of artemisinin in whole blood <1995JCH(B)183>. 

Supercritical fluid chromatography provides increased speed and resolution, relative to liquid chromatography, because of increased diffusion coefficients of solutes in supercritical fluids. (However, speed and resolution are slower than those of gas chromatography.) Unlike gases, supercritical fluids can dissolve nonvolatile solutes. When the pressure on the supercritical solution is released, the solvent turns to gas. leaving the solute in the gas phase for easy detection. Carbon dioxide is the supercritical fluid of choice for chromatography because it is compatible with flame ionization and ultraviolet detectors, it has a low critical temperature. and it is nontoxic. 

Edder et al. reported the capillary supercritical fluid chromatography of basic drugs of abuse, namely nicotine, caffeine, methadone, cocaine, imipramine, codeine, diazepam, morphine, benzoylecgonine, papverine, narcotine, and strychnine [25]. They compared the separation of these drugs on DBS and DB wax columns. The chromatographic conditions included a carbon dioxide mobile phase and a flame-ionization detector. It was noted that on the DBS column, all peaks other than methadone and cocaine were separated. With the exception of benzoylecgonine and papaverine, all other peaks were separated on a DB wax column. A reproducibility of less than 5% was obtained with an internal standard method. The detection limits obtained were within 10-50 ppm on both the columns. A linearity of >0.99 was obtained for methadone, codeine, and morphine in the concentration range 10-1000 ppm. 

Prednisolone has been analysed by capillary supercritical fluid chromatography in equine urine extract and was identified by matching retention time of pure standard. Supercritical fluid carbon dioxide was used as the mobile phase in conjunction with a methylpolysiloxane stationary phase capillary column and a flame ionization detector. SFC can thus be successfully applied for the estimation of prednisolone without derivatization (118). 

A major advantage of supercritical-fluid chromatography (SFC) is that it offers the advantage of liquid-like solubility, with the capability to use a nonselective gas-phase detector such as flame ionization detector. Other advantages of using supercritical fluids for extractions are that they are ine ensive, contaminant free, and less costly to dispose safely than organic solvents. 

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