Organic acids sample preparation

Regardless of sample type, the first step in our process is nucleic add amplification. The prestep is therefore nucleic acid extraction and/or purification and is highly dependent upon the sample type and matrix (blood, saliva, dirt, etc.) in which the organism(s) of interest is (are) found. Thus, nucleic acid sample preparation is somewhat outside the scope of our methods, but numerous kits and protocols are commercially available for various applications. Subsequent steps comprising PCR,... 

Carotenoid pigments were extracted by chloroform-acetone-isopropyl alcohol /2 l l/ after acetone extraction as described earlier. Lipids of different parts were extracted and their fatty acid composition were analysed by GLC. Tocopherols of different parts of the fruits were extracted, saponified and prepared for HPLC analysis according to Speek and co-workers. Organic acids were prepared by a method described previously. Following preparation the samples were redissolved in a minimal volume of the HPLC eluent. 

Investigated is the influence of the purity degree and concentration of sulfuric acid used for samples dissolution, on the analysis precision. Chosen are optimum conditions of sample preparation for the analysis excluding loss of Ce(IV) due to its interaction with organic impurities-reducers present in sulfuric acid. The photometric technique for Ce(IV) 0.002 - 0.1 % determination in alkaline and rare-earth borates is worked out. The technique based on o-tolidine oxidation by Ce(IV). The relative standard deviation is 0.02-0.1. 

Colorless phosphate ester surfactants were also prepared by treating P4O,0 with an organic OH-containing compound in the presence of a phosphinic acid color inhibitor, e.g., bis(hydroxymethyl)phosphinic acid color inhibitor. Thus, 558 parts dodecanol containing 2.4 parts of phosphinic acid color inhibitor was treated with 142 parts P4O10 at 100-135°C. The phosphate ester surfactant had a VCS color value of 1, whereas a sample prepared without the color inhibitor had a VCS color value of 5. Twenty-eight similar surfactants were prepared using various alcohols and alcohol-alkylene oxide condensates [22]. 

The analysis of a pharmaceutical tablet (6) requires sample preparation that is little more complex as most tablets contain excipients (a solid diluent) that may be starch, chalk, silica gel, cellulose or some other physiologically inert material. This sample preparation procedure depends on the insolubility of the excipient in methanol. As the components of interest are both acidic and neutral, the separation was achieved by exploiting both the ionic interactions between the organic acids and the adsorbed ion exchanger and the dispersive interactions with the remaining exposed reverse phase. 

Sample preparation Dried greater celandine was pulverized and briefly boiled in 0.05 mol sulfuric acid. After cooling to room temperature the mixture was placed in a separating funnel and adjusted to pH 10 with ammonia solution and extracted once with chloroform. The organic phase was dried with sodium sulfate and evaporated to dryness under reduced pressure. The residue was taken up in methanol and used as the sample solution for TLC. 

Because of their polymeric forms, alkylenebis(dithiocarbamates) are insoluble in water and most organic solvents. Additionally, they form strong complexes with different metal ions No extraction and chromatographic procedure has been reported for the parent compound of this chemical class. These compounds decompose readily under acidic conditions, for example by contact with the fruit or plant juice generated during sample preparation. 

Sample preparation for the common desorption/ionisation (DI) methods varies greatly. Films of solid inorganic or organic samples may be analysed with DI mass spectrometry, but sample preparation as a solution for LSIMS and FAB is far more common. The sample molecules are dissolved in a low-vapour-pressure liquid solvent - usually glycerol or nitrobenzyl alcohol. Other solvents have also been used for more specialised applications. Key requirements for the solvent matrix are sample solubility, low solvent volatility and muted acid - base or redox reactivity. In FAB and LSIMS, the special art of sample preparation in the selection of a solvent matrix, and then manipulation of the mass spectral data afterwards to minimise its contribution, still predominates. Incident particles in FAB and LSIMS are generated in filament ionisation sources or plasma discharge sources. 

DCP-AES can be used for high-viscosity matrices, slurries, etc. Organic solvents and acids can be handled without problems. Sample preparation is simpler than for ICP. Operating costs are much lower than for ICP-AES. Table 8.32 compares DCP-AES to ICP-AES and FAAS Table 8.33 shows typical detection limits. DCP and its applications were reviewed [208]. 

Sample preparation used to extract proteins from cells prior to analysis is an important step that can have an effect on the accuracy and reproducibility of the results. Proteins isolated from bacterial cells will have co-extracted contaminants such as lipids, polysaccharides, and nucleic acids. In addition various organic salts, buffers, detergents, surfactants, and preservatives may have been added to aid in protein extraction or to retain enzymatic or biological activity of the proteins. The presence of these extraneous materials can significantly impede or affect the reproducibility of analysis if they are not removed prior to analysis. 

Triprolidine hydrochloride in syrups and tablets can be analyzed by fluorimetry. A portion of the tablets or syrup is made basic with IN NaOH and extracted with ethylene chloride. The organic phase is then extracted with 0.1N I SO. The fluorescence of the acid extract is determined with a fluorometer using a UG11 filter for excitation and a Wratten 2A filter for emission. The fluorescence of the sample preparation is compared against a Reference Standard prepared in the same manner22. 

Sample preparation requires only dissolution of the sample to a suitable concentration in a mixture of water and organic solvent, commonly methanol, isopropanol, or acetonitrile. A trace of formic acid or acetic acid is often added to aid protonation of the analyte molecules in the positive ionization mode. In negative ionization mode ammonia solution or a volatile amine is added to aid deprotonation of the analyte molecules. 

SYNTHESIS A solution of 0.67 g 5-hydroxyindole (indol-5-ol) in 10 ml dry MeOH was treated with a solution of 0.30 g NaOMe in MeOH, followed by 0.70 g benzyl chloride. The mixture was heated on the steam bath for 0.5 h, and the solvent removed under vacuum. The residue was suspended between H20 and CH2CI2, the organic phase separated and the aqueous phase extracted once with CH2CI2. The combined organics were stripped of solvent under vacuum, and the residue distilled. A colorless fraction came over at 170-190 °C and spontaneously crystallized in the receiver. There was obtained 0.90 g (80%) 5-benzyloxyindole with a mp 81-86 °C which increased, on recrystallization from toluene / hexane, to 94-96 °C. A sample prepared from the decarboxylation of 5-benzyloxyindole-2-carboxylic acid has been reported to have a mp of 102 °C from benzene. 

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