Solid-phase extraction columns

Insufficient testing is one of the major causes of method failure. The amount of data needed to publish a new procedure in a peer-reviewed journal and the procedural detail supplied therein are often insufficient to allow a different user to validate a method rapidly. The developer should evaluate if the method will work using chemicals, reagents, solid-phase extraction columns, analytical columns, and equipment from various vendors. Separate lots of specific supplies within a vendor should be evaluated to determine if lot-to-lot variation significantly impacts method performance. Sufficient numbers of samples should be assayed to estimate the lifetime of the analytical column and to determine the effects of long-term use on the equipment. 

Liquid-liquid partitioning Solid-phase extraction Column chromatography... 

Mallat, E. and Barcelo, D., Analysis and degradation study of glyphosate and of aminomethylphosphonic in natural waters by means of polymeric and ion-exchange solid-phase extraction columns followed by ion chromatography-post-column derivatization with fluorescence detection, /. Chromatogr A, 823, 129, 1998. 

Recently, solid phase extraction (SPE) has been used to isolate members of this class of compounds. No solid phase support has been used exclusively and both hydrophobic- and hydrophilic-based solid phase extraction columns have been used for this assay. 

Water/SPM Collect water samples on disposable octyl-bonded silica solid-phase extraction columns dry elute with hexane/ether SPM collected by continuous flow centrifugation extract with acetone/water/benzene GC/ECD GC/MS O.lpg/L (water) 0.1 mg/kg (suspended particulate) 83 (water) 82 (suspended particulate) Ritsema et al. 1989... 

Green DR, Le Pape D. 1987. Stability of hydrocarbon samples on solid-phase extraction columns. Anal Chem 59 699-703. 

Other sulfonamides. The fact that the extraction of one of these sulfonamides is only optimized at a totally different pH displays the compilations in relying on a single set of extraction conditions as representative for all members within each class of PPCPs. To trap acid components in the sample, the sample has to be acidified to pH < 2, passed through a conditioned column such as an RP C18 solid-phase extraction column, and then eluted with a volatile solvent. Neutral compounds are, on the other hand, extracted by adjusting the sample to pH 7-8 before ranning the sample through the extraction column, which has been conditioned with acetone, methanol, or distilled water. Basic compounds are extracted by initially adjusting the sample to pH > 12 with EDTA and KOH. 

Cleanup of macrolides and lincosamides from coextracted material can also be accomplished with solid-phase extraction columns. Nonpolar sorbents such as XAD-2 resin (148) or reversed-phase sorbents (133, 134, 137, 141, 142) are usually employed in solid-phase extraction. In the latter case, ion-pairing with pentanesulfonic acid can also be applied for enhancing retention onto the hydro-phobic Ci8 material (154). However, these sorbents are not always effective for efficient cleanup of liver and kidney extracts. The basic character of macrolides and lincosamides suggests that cation-exchange sorbents such as aromatic-sulfonic acid (145,147), or polar sorbents such as silica (144,152,153), aminopropyl (139), or diol (149-151), can be powerful alternative approaches for isolation and/or cleanup of these compounds. 

Cleanup of nitro furans from coextracted substances and concentration of the extracts can also be accomplished with solid-phase extraction columns. Nonpolar sorbents such as reversed-phase (Cis) (37, 159-161, 170, 173, 177) or XAD-2 (178) materials are usually employed, since they provide high recovery of the analytes. However, in many cases, cleanup on these nonpolar sorbents is not effective in removing interfering substances from the extracts. Therefore, polar sorbents such as silica (29, 162), alumina (160, 179, 180), or aminopropyl (175, 176) materials are also frequendy employed as a more powerful alternative for extract cleanup. 

Cleanup and concentration of quinolones from coextracted matrix constituents can also be accomplished with solid-phase extraction columns that contain either nonpolar reversed-phase (Cis) sorbents (177, 197, 198), or polar sorbents such as alumina (189-191, 194), aminopropyl (182, 187), and propylsulfonic acid (188). Reversed-phase Cis material has also been employed as the sorbent in matrix solid-phase dispersion cleanup for the determination of oxolinic acid in catfish muscle (206). 

Elimination of coextracted materials and concentration of tetracyclines have also been accomplished using mixed-phase extraction membranes with both re-versed-phase and cation-exchange properties (294,295), or solid-phase extraction columns packed with cation-exchange materials such as CM-Sephadex C-25 (301), aromatic sulfonic acid (310), and carboxylic acid (283, 300). For the same purpose, metal chelate affinity chromatography has also been employed. In this technique, the tetracyclines are specifically absorbed on the column sorbent by chelation with copper ions bound to small chelating Sepharose fast flow column (278-281, 294-296). 

Cleanup by solid-phase extraction has also been widely employed since it is a simple, fairly inexpensive, and easy-to-perform procedure for purification of the crude extract. The use of disposable solid-phase extraction columns is currently part of most, if not all, modern analytical methods for the determination of anthelminthics in biological matrices at residue levels. Both normal-phase columns based on silica (333-335, 340, 367, 372), alumina (346, 373-375), or aminopropyl (339, 365, 370) materials, and reversed-phase columns based on Ci8 (319, 323, 324, 328, 344, 346, 347, 349-351, 357-359, 364, 367) and cyclohexyl (329, 332, 360) sorbents have been described in analytical applications. 

In some instances, combinations of normal- and reversed-phase columns can also be used for better purification of the crude extract. Combinations of Ci8 and alumina or Cig and silica solid-phase extraction columns have been successfully employed in the analysis of ivermectin residues in animal tissues (346) and bovine plasma (348), respectively. Elimination of coextracted materials and concentration of the analytes has also been accomplished using mixed-phase extraction columns. Such a copolymeric bonded silica column with both hydro-phobic and cationic functions has been employed in the analysis of hygromycin B in plasma, serum and milk (326). 

In some instances, combinations of Cig and silica columns are also used for better purification of the crude extracts (431, 445). A combination of Cg, silica, and amino solid-phase extraction columns has been successfully employed to fractionate anabolic and catabolic steroid hormone residues from meat in polar and nonpolar neutral and phenolic compounds, and to purify further each fraction effectively (452). Another combination of two solid-phase extraction columns, one using a graphitized carbon black sorbent and the other Amberlite resin in the hydroxyl form, allowed neutral anabolics to be isolated and separated from acidic anabolics and their metabolites (453). A combination of basic alumina column placed in tandem with an ion-exchange column has also been applied for the purification of the crude extracts in the determination of diethylstilbestrol and zeranol (427), and estradiol and zeranol in tissues (450). 

Solid-phase extraction columns offer a rough cleanup of the crude extract, which might nevertheless not be sufficient for some detection systems such as mass spectrometry. Some authors have proposed a combination of solid-phase extraction and liquid chromatography columns for extract cleanup (440). Other methods appeal to liquid chromatography on Cig columns with automated fraction collection. Fractions containing the analyte of interest were evaporated to dryness, yielding a residue that in most cases was suitable for gas chromatographic detection after suitable derivatization (445, 437). 

In contrast to liquid-liquid partitioning cleanup, which is particularly suitable for individual drugs or groups of drugs with similar chemical properties, solid-phase extraction is more appropriate for multiresidue analysis. On that account, solid-phase extraction in combination with liquid-liquid partitioning has become the method of choice in many laboratories for the purification of residues of sedatives and -blockers that may occur in biological matrices. Purification is usually accomplished on reversed-phase solid-phase extraction columns. Optimum retention of seven sedatives and carazolol on a reversed-phase solid-phase extraction column was reported when 10% sodium chloride solution was added to the acetonitrile hssue extract prior to its solid-phase extrachon cleanup (523, 524). A silica-based diol solid-phase extraction column was further suggested for efficient isolation of sedative and -blocker residues from food extracts (526). 

The 3 ml of new mixture is now passed on a disposable solid phase extraction column in order to separate the cyclosporins retained upon the sorbent. Following the rinsing and drying of the column, the cyclosporins are eluted with 1.5 ml of acetonitrile and are then concentrated to 200 pi following evaporation of solvent. A fraction of this final solution is injected into the chromatograph. 

Equipment and Instrumentation. Solid-phase extraction columns were obtained from J. T. Baker. Octadecyl (C18) and octyl (C8) 1-mL low-displacement columns were used as the primary extraction columns. Cyano and diol... 

Besides solid-phase extraction, column chromatography is also often used for cleanup and purification of polyphenolics from plant material. Ionic adsorbants (polyvinylpyrrolidone or PVP, polyamides, and Sephadex LH-20) and Amberlite XAD-2 resin have been used to isolate and purify polyphenolics from crude extracts. For the separation of polyphenolics from plant material, column chromatography using Sephadex LH-20, a gel-filtration matrix, is often used with various eluting solvents (Park and Lee, 1996). The most widely used solvents for column chromatography are aqueous methanol and aqueous ethanol. 

A novel multiresidue method has been developed for quantitation of TBZ, the metabolite 5-hydroxythiabendazole (5-OH-TBZ) in raw cow s milk. The 5-HS04-TBZ was hydrolyzed quantitatively under acidic conditions to 5-OH-TBZ. The TBZ and 5-OH-TBZ were extracted from milk at pH 8.0 with ethyl acetate, followed by cleanup of the extract on a cation-exchange solid-phase extraction column. Analytes were separated with a cation-exchange stationary phase ... 

J Slobodnik, AC Hogenboom, JJ Vreuls, JA Rontree, BLM van Baar, WM A Niessen, UAT Brinkman. Trace-level determination of pesticide residues using on-line solid-phase extraction-column liquid chromatography with atmospheric pressure ionization mass spectrometric and tandem mass spectrometric detection. J Chromatogr A 741 59-74, 1996. 

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