Sample preparation for chromatographic separations: an overview

Abstract Chromatographic methods dominate the field of organic analysis. However, many samples are too dilute, too complex or incompatible with the chromatographic system to render separation or detection possible without preliminary matrix simplification and/or preconcentration. A broad selection of the most common, recent and emerging isolation, clean-up and concentration techniques used to prepare samples for chromatographic separations are reviewed.

[1]  S. Hawthorne,et al.  Coupled SFE-GC: A Rapid and Simple Technique for Extracting, Identifying, and Quantitating Organic Analytes from Solids and Sorbent Resins , 1989 .

[2]  H. Langenhove,et al.  Comparison between theoretical and experimental sampling efficiencies on Tenax GC , 1985 .

[3]  J. Cooper,et al.  Automated sequential process for preparing samples for analysis by high-performance liquid chromatography. , 1987, Journal of chromatography.

[4]  A. Cecinato,et al.  Fractionation of polar polynuclear aromatic hydrocarbons present in industrial emissions and atmospheric samples and their determination by gas chromatography-mass spectrometry , 1986 .

[5]  T. A. Bellar,et al.  Determining volatile organics at microgram-per-litre levels by gas chromatography , 1974 .

[6]  Alberto J. Nún˜ez,et al.  Pre-concentration of headspace volatiles for trace organic analysis by gas chromatography , 1984 .

[7]  J. Namieśnik,et al.  Preconcentration of Atmospheric Terpenes on Solid Sorbents , 1985 .

[8]  P. Werkhoff,et al.  Dynamic headspace gas chromatography: concentration of volatile components after thermal desorption by intermediate cryofocusing in a cold trap : I. Principle and applications , 1987 .

[9]  T. Nestrick,et al.  Isomer-specific determination of chlorinated dioxins for assessment of formation and potential environmental emission from wood combustion , 1982 .

[10]  J. Sjövall,et al.  Gas chromatographic-mass spectrometric analysis of endogenous levels of estradiol in plasma and in cytosol from rat uterus. , 1982, Journal of chromatography.

[11]  C. Little,et al.  Increased sample throughput in HPLC using sample switching , 1984 .

[12]  B. Tomkins,et al.  Isolation of polycyclic organic compounds by solvent extraction with dimethyl sulfoxide , 1978 .

[13]  M. Saito,et al.  Simple microscale supercritical fluid extraction system and its application to gas chromatography-mass spectrometry of lemon peel oil , 1988 .

[14]  P. Wylie Headspace analysis with cryogenic focusing: A procedure for increasing the sensitivity of automated capillary headspace analysis , 1986 .

[15]  C. Cramers,et al.  A continuous preconcentration/extraction method for organic trace analysis by capillary gas chromatography , 1984 .

[16]  E. Hogendoorn,et al.  Liquid chromatographic determination of the fungicide iprodione in surface water, using on-line preconcentration. , 1985, The Science of the total environment.

[17]  A. Cecinato,et al.  Gas chromatographic evaluation of the organic components present in the atmosphere at trace levels with the aid of Carbopack B for pre-concentration of the sample , 1986 .

[18]  J. Pankow,et al.  Determination of volatile compounds in water by purging directly to a capillary column with whole column cryotrapping , 1988 .

[19]  K. Ramsteiner Systematic approach to column switching , 1988 .

[20]  A. Cappiello,et al.  Extraction of low molecular weight polynuclear aromatic hydrocarbons from ashes of coal-operated power plants. , 1987, Analytical chemistry.

[21]  J. Richard,et al.  Extraction of organic compounds from solid samples , 1986 .

[22]  K. Wahlund,et al.  Elimination of peak deformation in the liquid chromatographic separation of a strongly protein-bound drug from directly injected blood plasma samples. , 1983, Journal of chromatography.

[23]  A. Rustum Determination of acetaminophen in human plasma by ion-pair reversed-phase high-performance liquid chromatography. Application to a single-dose pharmacokinetic study. , 1989, Journal of chromatographic science.

[24]  A. C. Mehta Therapeutic monitoring of free (unbound) drug levels: Analytical aspects , 1989 .

[25]  J. Fritz,et al.  Concentration and determination of organic acids in complex aqueous samples , 1980 .

[26]  E. Hogendoorn,et al.  Pre-column clean-up and liquid chromatographic determination of residues of N-methylcarbamate pesticides in extracts of total diet. , 1987, Journal of Chromatography A.

[27]  G. Senum Theoretical collection efficiencies of adsorbent samplers. , 1981, Environmental science & technology.

[28]  A. M. Gillespie,et al.  HPLC Silica Column Fractionation of Pesticides and PCB from Butterfat , 1986 .

[29]  G. MacLeod,et al.  Comparative assessment of the artefact background on thermal desorption of tenax GC and tenax TA , 1986 .

[30]  K. Grob,et al.  Determination of free and esterified sterols and of wax esters in oils and fats by coupled liquid chromatography-gas chromatography , 1989 .

[31]  K. Ganzler,et al.  Microwave extraction. A novel sample preparation method for chromatography. , 1986, Journal of chromatography.

[32]  U. Brinkman,et al.  Monitoring of veterinary drug residues by a combination of continuous flow techniques and column-switching high-performance liquid chromatography. I. Sulphonamides in egg, meat and milk using post-column derivatization with dimethylaminobenzaldehyde. , 1988, Journal of chromatography.

[33]  J. Drozd,et al.  Headspace gas analysis by gas chromatography , 1979 .

[34]  C. Bicchi,et al.  Improved method for the analysis of small amounts of essential oils by microdistillation followed by capillary gas chromatography , 1983 .

[35]  Cecilia C. Chan,et al.  Sample Handling and Analysis for 51 Volatile Organics by an Adapted Purge and Trap GC-MS Technique , 1987 .

[36]  S. Berkowitz Linear Multidimensional Liquid Chromatography in Protein Separation , 1987 .

[37]  T. Alsberg,et al.  Vacuum sublimation and solvent extraction of polycyclic aromatic compounds adsorbed on carbonaceous materials , 1981 .

[38]  J. King Fundamentals and Applications of Supercritical Fluid Extraction in Chromatographic Science , 1989 .

[39]  E. Bargar Application of column switching in high-performance liquid chromatographic analysis of medroxalol in plasma. , 1987, Journal of chromatography.

[40]  B. Wenclawiak,et al.  Direct on-line coupling of small subcritical and supercritical fluid extractors with packed column supercritical fluid chromatography , 1988 .

[41]  R. W. Frei,et al.  Trace enrichment of polar compounds on chemically bonded and carbonaceous sorbents and application to chlorophenol , 1981 .

[42]  Stephen G. Walburn,et al.  Collection and analysis of hazardous organic emissions , 1982 .

[43]  G. V. Calder,et al.  Use of macroreticular resins in the analysis of water for trace organic contaminants. , 1974, Journal of chromatography.

[44]  D. Underhill,et al.  Fundamental factors in the performance of diffusive samplers , 1989 .

[45]  T. Peters Steam distillation apparatus for concentration of trace water soluble organics , 1980 .

[46]  R. Macdonald,et al.  Measurement of natural trace dissolved hydrocarbons by in situ column extraction. An intercomparison of two adsorption resins , 1989 .

[47]  R. Melcher,et al.  Sampling and sample preparation of environmental material , 1986 .

[48]  G. Verga,et al.  Direct headspace gas chromatography with fused-silica capillary columns and multiple simultaneous detection , 1983 .

[49]  J. A. Perry,et al.  Separation of furosemide, phenylbutazone and oxyphenbutazone in plasma by direct injection onto internal surface reversed-phase columns with systematic optimization of selectivity. , 1986, Journal of chromatography.

[50]  L. Ettre,et al.  Investigations on Equilibrium Headspace — Open Tubular Column Gas Chromatography , 1980 .

[51]  E. Pellizzari,et al.  Chemical transformations during ambient air sampling for organic vapors , 1984 .

[52]  K. Unger,et al.  On-line high-pressure extraction-high-performance liquid chromatography , 1983 .

[53]  R. E. Kepner,et al.  Freeze concentration of volatile components in dilute aqueous solutions. , 1969, Journal of agricultural and food chemistry.

[54]  T. Pinkerton,et al.  Internal surface reversed-phase silica support prepared with chymotrypsin , 1986 .

[55]  T. Peters Comparison of continuous extractors for the extraction and concentration of trace organics from water , 1982 .

[56]  D. K. Chow,et al.  Compounds Resistant to Carbon Adsorption in Municipal Wastewater Treatment , 1977 .

[57]  R. H. Brown,et al.  Collection and analysis of trace organic vapour pollutants in ambient atmospheres , 1979 .

[58]  F. Poy,et al.  Determination of vinyl chloride monomer residue in poly(vinyl chloride) at the parts-per-billion level with an automatic purge-and-trap technique. , 1987, Journal of chromatography.

[59]  P. Sandra,et al.  New method for quantitative essential oil analysis , 1981 .

[60]  K. Grob,et al.  Stripping of trace organic substances from water: Equipment and procedure , 1976 .

[61]  J. Albaigés,et al.  Organic Pollutants in Water. I. Optimization of Operational Parameters of he CLSA Technique , 1987 .

[62]  H. Neukom,et al.  Coupling of high-performance liquid chromatography with capillary gas chromatography , 1984 .

[63]  D. Hughes Recovery factor for extraction from a solid, extractant-retaining matrix , 1983 .

[64]  L. Ng Sample preparation by salts precipitation and quantitation by high-performance liquid chromatography with UV detection of selected drugs in biological fluids. , 1983, Journal of chromatography.

[65]  G. Hunt,et al.  Potential contamination from the use of synthetic adsorbents in air sampling procedures , 1982 .

[66]  H. Svec,et al.  Liquid-liquid fractionation of complex mixtures of organic components , 1981 .

[67]  D. Hunt,et al.  Analysis of nitrated polycyclic aromatic hydrocarbons in diesel particulates , 1982 .

[68]  J. T. Swanson,et al.  Supercritical Fluid Extraction as a Sample Introduction Method for Chromatography , 1989 .

[69]  P. Donkin,et al.  Application of steam distillation in the determination of petroleum hydrocarbons in water and mussels (Mytilus edulis) from dosing experiments with crude oil , 1984 .

[70]  T. Bellar,et al.  Interlaboratory study on determination of polychlorinated biphenyls in environmentally contaminated sediments , 1985 .

[71]  D. Underhill,et al.  Estimating contaminant concentration from uptake on a diffusive sampler , 1989 .

[72]  D. Westerlund Direct injection of plasma into column liquid chromatographic systems , 1987 .

[73]  W. Bertsch,et al.  Evaluation of sampling methods for the determination of trace organics in water , 1983 .

[74]  R. G. Webb Solvent Extraction of Organic Water Pollutants , 1978 .

[75]  Milton L. Lee,et al.  Standardization of alumina and silica adsorbents used for chemical class separations of polycyclic aromatic compounds , 1985 .

[76]  E. Morgan,et al.  Versatile microreactor and extractor , 1986 .

[77]  D. Murray Rapid micro extraction procedure for analyses of trace amounts of organic compounds in water by gas choromatography and comparisons with macro extraction methods , 1979 .

[78]  J. Curvers,et al.  Possibilities and limitations of steam distillation—extraction as a pre-concentration technique for trace analysis of organics by capillary gas chromatography , 1983 .

[79]  C. Poole,et al.  Preparation of environmental samples for the determination of polycyclic aromatic hydrocarbons by thin-layer chromatography. , 1987, Journal of chromatography.

[80]  C. Cramers,et al.  Possibilities and limitations of dynamic headspace sampling as a pre-concentration technique for trace analysis of organics by capillary gas chromatography , 1984 .

[81]  J. Rudolph,et al.  Problems connected with the analysis of halocarbons and hydrocarbons in the non-urban atmosphere. , 1986, International journal of environmental analytical chemistry.

[82]  L. Tuinstra,et al.  Universal extraction/clean-up procedure for screening of pesticides by extraction with ethyl acetate and size exclusion chromatography , 1987 .

[83]  E. Delwiche,et al.  Large-scale semicontinuous solid-liquid extraction apparatus , 1982 .

[84]  M. Wells,et al.  Reversed-phase solid-phase extraction for aqueous environmental sample preparation in herbicide residue analysis , 1987 .

[85]  R. G. Lewis,et al.  Passive sampling devices with reversible adsorption , 1985 .

[86]  B. W. Wright,et al.  On-line supercritical fluid extraction-capillary gas chromatography , 1987 .

[87]  Paul T. Williams,et al.  On-line fractionation and identification of diesel fuel polycyclic aromatic compounds by two-dimensional microbore high-performance liquid chromatography/capillary gas chromatography , 1988 .

[88]  Konrad Grob,et al.  On-line coupled high-performance liquid chromatography—gas chromatography , 1989 .

[89]  H. Yoshida,et al.  High-performance liquid chromatographic drug analysis by direct injection of whole blood samples. II. Determination of hydrophilic drugs. , 1987, Journal of chromatography.

[90]  M. Dressler Extraction of trace amounts of organic compounds from water with porous organic polymers , 1979 .

[91]  R. W. Frei,et al.  Automated pre-column system for trace enrichment and clean-up of plasma samples in narrow-bore liquid chromatography , 1985 .

[92]  F. Onuska,et al.  Supercritical fluid extraction of 2,3,7,8‐tetrachlorodibenzo‐p‐dioxin from sediment samples , 1989 .

[93]  W. Giger,et al.  Determination of trace levels of phenol and cresols in rain by continuous liquid-liquid extraction and high-performance liquid chromatography. , 1987, Journal of chromatography.

[94]  G. W. Wooten,et al.  Thermally desorbable passive sampling device for volatile organic chemicals in ambient air , 1985 .

[95]  J. Richard,et al.  Organics in water: solid phase extraction on a small scale , 1988 .

[96]  I. Suffet,et al.  Evaporative concentration system for trace organic analysis , 1987 .

[97]  S. Wise,et al.  Characterization of the Polycyclic Aromatic Hydrocarbons from Two Standard Reference Material Air Particulate Samples , 1986 .

[98]  R. Rosset,et al.  Synthesis of silver and copper(II) silica gels for the liquid chromatograpic separation of olefinic hydrocarbons in the group analysis of light and heavy petroleum compounds , 1987 .

[99]  F. Janssen,et al.  Trace analysis of halogenated hydrocarbons in gaseous samples by on-line enrichment in an adsorption trap, on-column cold-trapping and capillary gas chromatography. I.Method and instrumentation , 1987 .

[100]  S. C. Ruckmick,et al.  Liquid chromatographic systems for the separation of polycyclic aromatic hydrocarbon and nitrogen heterocycle compounds present in coal liquids , 1985 .

[101]  U. Juergens High-performance liquid chromatographic determination of antiepileptic drugs by an advanced automated sample processor. , 1986, Journal of chromatography.

[102]  R. Chalmers,et al.  Studies on the quantitative freeze-drying of aqueous solutions of some metabolically important aliphatic acids prior to gas-liquid chromatographic analysis. , 1972, In Analysis.

[103]  Y. Shimoishi Some 1,2-diaminobenzene derivatives as reagents for gas chromatographic determination of selenium with an electron-capture detector. , 1977, Journal of chromatography.

[104]  J. F. Lawrence Analytical methodology for organophosphorus pesticides used in Canada. , 1987, International journal of environmental analytical chemistry.

[105]  J. Tanaka,et al.  Comparison of solvent reduction methods for concentration of polycyclic aromatic hydrocarbon solutions , 1984 .

[106]  J. Duinker,et al.  Clean-up of environmental samples by high-performance liquid chromatography for analysis of organochlorine compounds by gas chromatography with electron-capture detection. , 1988, Journal of chromatography.

[107]  J. Pankow,et al.  Assessment of adsorption/solvent extraction with polyurethane foam and adsorption/thermal desorption with Tenax-GC for the collection and analysis of ambient organic vapors , 1985 .

[108]  E. Peltzer,et al.  Sampling and quantitation of lipids in aerosols from the remote marine atmosphere , 1987 .

[109]  J. Shapiro Concentration of volatile substances in aqueous solution and production of water free of organics by freezing out , 1967 .

[110]  Toshiyuki Tanaka Chromatographic characterization of porous polymer adsorbents in a trapping column for trace organic vapor pollutants in air , 1978 .

[111]  V. Lopez-Avila,et al.  Determination of 51 priority organic compounds after extraction from standard reference materials , 1983 .

[112]  A. Zlatkis,et al.  The role of organic volatile profiles in clinical diagnosis. , 1981, Clinical chemistry.

[113]  R. Majors Multidimensional High Performance Liquid Chromatography , 1980 .

[114]  R. W. Frei,et al.  Use of Pyrocarbon Sorbents for Trace Enrichment of Polar Compounds from Aqueous Samples with On-line HPLC Analysis , 1983 .

[115]  J. Fritz,et al.  Simple steam distillation for sample preparation prior to gas chromatographic determination of organic compounds , 1987 .

[116]  M. McNally,et al.  Supercritical fluid extraction coupled with supercritical fluid chromatography for the separation of sulfonylurea herbicides and their metabolites from complex matrices. , 1988, Journal of chromatography.