Extract preparation procedure

Theoretical and applied aspects of microwave heating, as well as the advantages of its application are discussed for the individual analytical processes and also for the sample preparation procedures. Special attention is paid to the various preconcentration techniques, in part, sorption and extraction. Improvement of microwave-assisted solution preconcentration is shown on the example of separation of noble metals from matrix components by complexing sorbents. Advantages of microwave-assisted extraction and principles of choice of appropriate solvent are considered for the extraction of organic contaminants from solutions and solid samples by alcohols and room-temperature ionic liquids (RTILs). 

Prepare a blank solution by carrying through all the sequences of the separation procedures using a hydrochloric acid solution to which no alloy has been added, and then measure the absorption given by this blank solution, by a series of standard solutions containing from 1 to 10 /rg Pb mL 1 prepared by suitable dilution of the lead caprate stock solution (see Note), and finally of the extract prepared from the sample of alloy. Plot the calibration curve and determine the lead content of the alloy. 

Calibration data (e.g., linearity or sensitivity) are not discussed in detail between laboratories, but a typical calibration starts with 50% of the lowest fortification level and requires at least three additional calibration levels. Another point of calibration is the use of appropriate standards. In 1999 a collaborative study tested the effect of matrix residues in final extracts on the GC response of several pesticides.Five sample extracts (prepared for all participants in one laboratory using the German multi-residue procedure) and pure ethyl acetate were fortified with several pesticides. The GC response of all pesticides in all extracts was determined and compared with the response in the pure solvent. In total, 20 laboratories using 47 GC instruments... 

Ivermectin, a macrocyclic lactone, is also utilized to control parasites. An immunoassay was developed to determine ivermectin residues in bovine liver by Crooks etal. The sample preparation procedure was complex, involving tissue homogenization in acetonitrile, centrifugation, extraction with hexane (to remove lipids), evaporation and reconstitution in ethyl acetate, and passage through an SPE column followed... 

Sample preparation consists of homogenization, extraction, and cleanup steps. In the case of multiresidue pesticide analysis, different approaches can have substantially different sample preparation procedures but may employ the same determinative steps. For example, in the case of soil analysis, the imidazolinone herbicides require extraction of the soil in 0.5 M NaQH solution, whereas for the sulfonylurea herbicides, 0.5M NaOH solution would completely decompose the compounds. However, these two classes of compounds have the same determinative procedure. Some detection methods may permit fewer sample preparation steps, but in some cases the quality of the results or ruggedness of the method suffers when short cuts are attempted. For example, when MS is used, one pitfall is that one may automatically assume that all matrix effects are eliminated because of the specificity and selectivity of MS. 

SFE usually requires pre-extraction manipulation in the form of cryogenic grinding, except in cases where analytes are sorbed only on the surface or outer particle periphery. The optimum particle diameter is about 10-50 p,m. Diatomaceous earth is used extensively in SFE sample preparation procedures. This solid support helps to disperse the sample evenly, allowing the SCF to solvate the analytes of interest efficiently and without interference from moisture. 

Table 3.4 contains a comparison of microwave extraction with other sample preparation procedures. MAE compares favourably with Soxhlet/Soxtec and... 

Klink [135] recently discussed sample preparation procedures for LC-MS. SPE can be so well integrated into the concept of LC-MS, that in many automated applications no clear distinction exists between SPE and LC [135]. In on-line LC-MS mode, the possibilities for changing the eluent are rather limited, because of the tolerance of the eluent for the interface. Moreover, the conventional gradient mode may lead to strong fluctuations in the response of the MS detector. Here the off-line mode, using SPE for concentration followed by selective elution, enables very far-reaching preseparation, due to the differences in the polarity of the eluents applied and their mixtures. Although the overall benefits of SPE for LC-MS applications are positive, extracts... 

In order to prepare the methoxychlor for analysis, it must be removed from the material under examination by means of a solvent extraction. The procedures used for the stripping of DDT are applicable to methoxychlor (2, 5, 6). The solvent chosen should readily dissolve methoxychlor, be sufficiently volatile to be evaporated by an air current at room temperature, and leave no residue upon evaporation that will interfere with the analysis. 

Wang et al. also addressed the mass spectral reproducibility. They conducted a carefully controlled interlaboratory experiment where the effects of a number of parameters were systematically investigated.22 They demonstrated that nearly identical spectra could be obtained in carefully controlled experiments. Minor variations in the sample/matrix preparation procedures for MALDI and in the experimental conditions used for bacterial protein extraction or analysis were shown to result in changes in the resulting spectra. They also noted that a subset of peaks was less sensitive to experimental variables. These ions appeared to be conserved in spectra obtained even under different experimental conditions so long as they were obtained using genetically identical bacteria. The existence of these conserved peaks helped explain... 

Generally it is not possible to introduce a material, e.g. a piece of ceramic, as it is, into a mass spectrometer an appropriate sample preparation procedure, basically consisting of analytes extraction from the substrates and in their preliminary purification, precedes the mass spectrometric analysis. 

These samples are prepared by either wet or dry ashing. Many of the metals can be determined in aqueous solution, but for the more trace ones, solvent extraction procedures similar to those described above are resorted to. Similar sample preparation procedures apply to plants. The elements... 

Recovery — Recovery control (RC) solutions were prepared in 10/90 v/v ACN/water. Recovery evaluation (RE) samples were prepared in human plasma. Aliquot of RC solutions into assay plates followed sample preparation procedure steps 1 and 2. Instead of adding 50 pL of diluent, wells containing RC solutions were dried down under a steady stream of room temperature N2. The dried wells were then reconstituted with 250 pL of diluent. Reconstituted RC solutions were directly injected onto an HPLC analytical column, bypassing the extraction column. RE samples were aliquoted into an assay plate following normal sample preparation. RE samples were analyzed using the full extraction procedure (with extraction column). The analyte was tested at three concentration levels and the internal standard was tested at one. Mean extraction recovery for fenofibric acid varied from 93.2 to 111.1%, and mean extraction recovery for the Pestanal internal standard was 105.2%. 

The most common (off-line) sample preparation procedures after protein precipitation are solid phase extraction and liquid-liquid extraction. Multiple vendors and available chemistries utilize 96-well plates for solid phase extraction systems and liquid-liquid extraction procedures. Both extraction process can prepare samples for HPLC/MS/MS assay. Jemal et al.110 compared liquid-liquid extraction in a 96-well plate to semi-automated solid phase extraction in a 96-well plate for a carboxylic acid containing analyte in a human plasma matrix and reported that both clean-up procedures worked well. Yang et al.111 112 described two validated methods for compounds in plasma using semi-automated 96-well plate solid phase extraction procedures. Zimmer et al.113 compared solid phase extraction and liquid-liquid extraction to a turbulent flow chromatography clean-up for two test compounds in plasma all three clean-up approaches led to HPLC/MS/MS assays that met GLP requirements. 

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