Extraction procedures liquid chromatography

Following the primary sample extraction, the crude extract can be further subjected to various types of cleanup procedures including conventional liquid-liquid partitioning, solid-phase extraction, and liquid chromatography cleanup. In some instances, more than one of these cleanup procedures may be used in combination to obtain highly purified extracts. 

The extraction procedure for A -THC, as revealed by experiments with / H /-A -THC, is quite efficient and the recovery after both extraction and liquid chromatography is usually over 80%. 

High performance liquid chromatography (HPLC) has been by far the most important method for separating chlorophylls. Open column chromatography and thin layer chromatography are still used for clean-up procedures to isolate and separate carotenoids and other lipids from chlorophylls and for preparative applications, but both are losing importance for analytical purposes due to their low resolution and have been replaced by more effective techniques like solid phase, supercritical fluid extraction and counter current chromatography. The whole analysis should be as brief as possible, since each additional step is a potential source of epimers and allomers. 

A UV spectrum with a pronounced absorption above 210 nm allows UV detection after liquid chromatography (LC), but an absorption maximum in the range of visible light may also decompose during cleanup procedures and require the elimination of light when handling extracts. 

The enforcement methods provided by the applicants give basic information about appropriate cleanup steps and specific determination procedures. Typically, direct use of this developmental work occurred when a GC multi-residue method was found appropriate. Owing to the recent developments in the field of MS/MS with atmospheric pressure ionization, an alternative approach for those compounds that can be analyzed by liquid chromatography (LC) will soon be possible. It is important that some fundamental considerations for such method(s) should be agreed at the outset. Considerations include the most suitable extraction solvents and cleanup steps and some standard HPLC conditions. 

Specifically for triazines in water, multi-residue methods incorporating SPE and LC/MS/MS will soon be available that are capable of measuring numerous parent compounds and all their relevant degradates (including the hydroxytriazines) in one analysis. Continued increases in liquid chromatography/atmospheric pressure ionization tandem mass spectrometry (LC/API-MS/MS) sensitivity will lead to methods requiring no aqueous sample preparation at all, and portions of water samples will be injected directly into the LC column. The use of SPE and GC or LC coupled with MS and MS/MS systems will also be applied routinely to the analysis of more complex sample matrices such as soil and crop and animal tissues. However, the analyte(s) must first be removed from the sample matrix, and additional research is needed to develop more efficient extraction procedures. Increased selectivity during extraction also simplifies the sample purification requirements prior to injection. Certainly, miniaturization of all aspects of the analysis (sample extraction, purification, and instrumentation) will continue, and some of this may involve SEE, subcritical and microwave extraction, sonication, others or even combinations of these techniques for the initial isolation of the analyte(s) from the bulk of the sample matrix. 

Using a simple solvent extraction procedure to minimize matrix effects, a diclofop-methyl immunoassay was developed for milk, a number of edible plant products, and other matrices. Gas chromatography (GC) and liquid scintillation counting (LSC) of a C-labeled analyte were used as reference methods to compare with enzyme immunoassay (EIA) results. The methods were well correlated, with comparison of EIA... 

The concept of SPME was first introduced by Belardi and Pawliszyn in 1989. A fiber (usually fused silica) which has been coated on the outside with a suitable polymer sorbent (e.g., polydimethylsiloxane) is dipped into the headspace above the sample or directly into the liquid sample. The pesticides are partitioned from the sample into the sorbent and an equilibrium between the gas or liquid and the sorbent is established. The analytes are thermally desorbed in a GC injector or liquid desorbed in a liquid chromatography (LC) injector. The autosampler has to be specially modified for SPME but otherwise the technique is simple to use, rapid, inexpensive and solvent free. Optimization of the procedure will involve the correct choice of phase, extraction time, ionic strength of the extraction step, temperature and the time and temperature of the desorption step. According to the chemical characteristics of the pesticides determined, the extraction efficiency is often influenced by the sample matrix and pH. 

Residue analytical methods for neonicotinoids in crops, soil and water samples have been developed. The basic principle of these methods consists of the following steps extraction of the crop and/or soil samples with acetone or the other organic solvent, cleanup by liquid-liquid partition or column chromatography, and quantitative analysis by high-performance liquid chromatography with ultraviolet detection (HPLC/UV). Simple column cleanup procedures are used to improve the accuracy and sensitivity of these methods. 

Crop material is homogenized with acetonitrile-water (9 1, v/v). The crop extract is centrifuged and an aliquot is rotary evaporated to a small volume. The sample is subjected to a Cig solid-phase extraction (SPE) cleanup procedure. The concentrated eluate is subjected to liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis. 

This procedure was compared with sequential extractive techniques employing alkaline hydrolysis of dried plant tissue followed by extraction of the acidified mixture with ethyl acetate. Fractions were individually evaluated for phytotoxic properties. Selected fractions from those showing a positive response were analyzed by gas-liquid chromatography. Structural identification and characterization of the individual components in these selected fractions were accomplished by gas chromatography-mass spectrometry. 

Dye identification is of great interest in textile studies. The classical procedure requires a hydrolysis step and other extraction techniques, followed by identification of the individual compounds present after separation by a chromatographic technique, e.g. high-performance liquid chromatography [Novotna et al. 1999, Szostek et al. 2003]. However, ToF-SIMS can be an alternative method, avoiding the phase of extraction which is always a time consuming and delicate step because of the possible destruction of the molecular structure of the sample [Ferreira et al. 2002]. The development of ToF-SIMS for dye detection has been reported in different studies. 

Liquid chromatography is the core preparative technique in protein purification, and all supplementary procedures like extraction, centrifugation and filtration, ultimately serve to condition the protein solution for chromatography. A series of chromatographic steps, usually termed capture, intermediate purification and polishing, mak-... 

Brown and Rhead [307] improved the sensitivity of high-performance liquid chromatography to 0.2 xg/l. This procedure consists ofbromination, extraction of the a, /i-dibromopropionamide with ethyl acetate, and quantification using high-performance liquid chromatography with ultraviolet detection. Samples... 

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