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At least 19 recordsLinked to original sources

Comparison of the chromatographic properties of sterols, select additional steroids and triterpenoids: gravity-flow column liquid chromatography, thin-layer chromatography, gas-liquid chromatography and high-performance liquid chromatography.

The chromatographic properties of approximately 100 sterols, select steroids of plant origin (sapogenins and steroidal alkaloids) and triterpenoids has been evaluated in this laboratory by monitoring their elution characteristics in adsorption (gravity column and thin-layer methods with and without the addition of silver nitrates), gas and reversed-phase high-performance liquid chromatography. The utility of each methodology to act in one or another chromatographic mode-separation, radio-chemical purification, quantitation and structural elucidation, is discussed. The importance of the tilt of the -OH group at C-3 as well as the polarity, size, an shape of the rest of the molecule as it effects the hydrogen-bonding ability of the -OH group is demonstrated through changes in chromatographic behavior that result from the step-wise introduction of double bonds, methyl, bromo, oxygen, nitrogen and cyclopropyl groups into 5 alpha-cholestanol. An independent aid in the structure identification and quantitation of the compounds was use of a multiple-wavelength diode array detector in which different wavelengths of the UV spectrum (200-400 nm) were simultaneously monitored following passage of the sample through a reversed-phase C18 column.

Chromatography, Gas↗

Midazolam determination by gas chromatography, liquid chromatography and gas chromatography--mass spectrometry.

Midazolam is determined in serum by gas chromatography with a nitrogen-selective detector, by liquid chromatography, and by gas chromatography--mass spectrometry. Comparable results are obtained with the three techniques with a within-run precision of 9% by gas chromatography and gas chromatography---mass spectrometry and 5% by liquid chromatography. Between-run precision is 13% by gas chromatography--mass spectrometry and 10% by liquid chromatography. Comparison of patient's sera by gas chromatography (x), liquid chromatography (y), and by gas chromatography (x), gas chromatography--mass spectrometry (y) gave correlations of 0.98 and 0.89, respectively. Interferences observed when using one technique, for example liquid chromatography, can be eliminated by analyzing the sample extract with one of the other techniques.

Anti-Anxiety Agents↗

Disopyramide determination by gas chromatography, liquid chromatography, and gas chromatography--mass spectrometry.

Disopyramide is determined in serum by gas chromatography with a nitrogen-selective detector, by liquid chromatography, and by gas chromatography--mass spectrometry. Comparable results are obtained with the three techniques, with a within-run and between-run precision of 5 to 10% (coefficient of variation). Least-squares analysis of data on patients' sera, analyzed first by gas chromatography (y) and then liquid chromatography (x), gave a slope of 1.12; y-intercept, -0.31; standard error of estimate, 0.46; and correlation coefficient, 0.94. Comparison of patients' sera by gas chromatography (y) and then by gas chromatography--mass spectrometry (x) gave a slope of 0.94; y-intercept, 0.42; standard error of estimate, 0.38; and correlation coefficient, 0.97. Interferences observed when using one technique--for example, gas chromatography--can be eliminated by analyzing the sample extract with one of the other techniques.

Chromatography, Gas↗

Rational methods for predicting human monoclonal antibodies retention in protein A affinity chromatography and cation exchange chromatography. Structure-based chromatography design for monoclonal antibodies.

Rational methods for predicting the chromatographic behavior of human monoclonal antibodies (hMabs) in protein A affinity chromatography and cation exchange chromatography from the amino acid sequences information were proposed. We investigated the relation between the structures of 28 hMabs and their chromatographic behavior in protein A affinity chromatography and cation exchange chromatography using linear gradient elution experiments. In protein A affinity chromatography, the elution pH of the hMabs was correlated with not only the structure of the Fc region (subclass), but also that of the variable region. The elution pH of hMabs that have LYLQMNSL sequences in between the CDR2 and CDR3 regions of the heavy chain became lower among the same subclass of hMabs. In cation exchange chromatography, the peak salt concentrations IR of hMabs that have the same sequences of variable regions (or that have a structural difference in their Fc region, which puts them into a subclass) were similar. The IR values of hMabs were well correlated with the equilibrium association constant Ke, and also with the surface positive charge distribution of the variable region of the heavy chain (corrected surface net positive charge (cN) of the VH region). Based on these findings, we developed rational methods for predicting the retention behavior, which were also tested with eight additional hMabs. By considering the information on the number of binding sites associated with protein adsorption as determined experimentally, and the surface positive charge distribution from the three-dimensional structure of Mab A, we hypothesized that hMabs is separated by cation exchange chromatography as the surface positive charge distribution of the VH region is recognized.

Amino Acid Sequence↗

Separation of stereoisomers of several furan derivatives by capillary gas chromatography-mass spectrometry, supercritical fluid chromatography, and liquid chromatography using chiral stationary phases.

The direct separation of several stereoisomers (enantiomers and geometrical isomers) of furan derivatives, important intermediates for the synthesis of physiologically active natural products, was achieved using capillary gas chromatography/mass spectrometry with a per-O-methyl-beta-cyclodextrin, supercritical fluid chromatography and high-performance liquid chromatography with a tris(3,5-dimethylphenylcarbamate) of cellulose or amylose for the chiral stational phases, respectively. The temperature dependence of the peak resolution (Rs) and the retention factor (k) over the range of 110-130 degrees was studied using crotyl furfuryl ether in gas chromatography. Successive increases in the Rs value and of the difference between the k value of the E-isomer and the k value of the Z-isomer were observed when the gradient temperature was decreased. The per-O-methyl-beta-cyclodextrin column was suitable for use with volatile furan ethers whose molecular masses are between 150 and 180. In conclusion, the separation of thermally unstable furan derivatives was accomplished using supercritical fluid chromatography and high-performance liquid chromatography.

Chromatography, High Pressure Liquid↗

Estradiol-17 beta quantified in serum by isotope dilution-gas chromatography-mass spectrometry: reversed-phase C18 high-performance liquid chromatography compared with immuno-affinity chromatography for sample pretreatment.

Here, isotope dilution-gas chromatography-mass spectometry is used as a reference technique for determining the concentration of estradiol-17 beta in candidate human serum Reference Material. The accuracy of assigned concentrations in biologic materials is not only determined by instrumental performance, it also depends greatly on the selectivity of the procedure for isolating the analyte from the biological matrix, an issue which we consider insufficiently addressed in the literature. We introduced reversed-phase C18 high-performance liquid chromatography as a fractionation procedure in addition to the commonly used solvent extraction and column chromatography on Sephadex LH-20. The validity of this approach as part of a Reference Method for measurement of estradiol-17 beta by isotope dilution-gas chromatography-mass spectrometry was investigated by comparison with immuno-affinity chromatography, which on theoretical grounds is generally considered as highly selective.

Chromatography, Affinity↗

Method for characterization of selectivity in reversed-phase liquid chromatography. III. Retention behaviour in gradient-elution chromatography: application to the chromatography of pesticide compounds.

The method introduced recently for the characterization and prediction of absolute and relative retention in reversed-phase liquid chromatography under isocratic conditions has been applied to gradient-elution chromatography. The method is based on two indices (one lipophilic, nce, and the other polar, qi, to characterize the behaviour of each solute in methanol-water mobile phases of various compositions. The indices nce and qi of phenylurea and triazine herbicides were found to be composed of additive contributions of structural elements (functional groups) in the molecules of the solutes. Using the present approach, it is possible to predict retention volumes in gradient-elution chromatography with a precision comparable to those under isocratic conditions (i.e., less than 10% relative for most compounds tested). Simultaneous adjustment of the initial mobile phase composition and the slope of the linear gradient makes it possible to control to a certain extent the selectivity in gradient-elution chromatography using binary solvent gradients and offers an alternative approach to the use of multi-solvent gradients for selectivity control. This method may be especially useful in optimizing gradient-elution separations of pairs of compounds with positive differences in both indices nce and qi, delta nce greater than 0 and delta q greater than 0. Selection of the optimal gradient profile is illustrated on a practical example of gradient-elution chromatography of phenylurea herbicides.

Chromatography, Liquid↗

Determination of organophosphorus pesticides in fruits by on-line size-exclusion chromatography-liquid chromatography-gas chromatography-flame photometric detection.

The determination of organophosphorus pesticides in fruits by size-exclusion chromatography (SEC) on a polystyrene column coupled on-line to a gas chromatography (GC) system was unsatisfactory as a result of interfering peaks in GC. A liquid chromatography step on silica gel was therefore inserted between the SEC and GC steps to filter out polar by-products. Samples of fruit (apples, grapes and kiwi fruits) were extracted, then the extract filtered or centrifuged and injected into an automated on-line SEC-liquid chromatography-GC-flame photometric detection. Recoveries were about 95% and the detection limits about 1 ng/g.

Chromatography, Gas↗

Application of liquid chromatography-mass spectrometry analysis in metabolomics: reversed-phase monolithic capillary chromatography and hydrophilic chromatography coupled to electrospray ionization-mass spectrometry.

Analysis of the entire metabolome as the sum of all detectable components in the sample rather than analysis of each individual metabolite is performed by the metabolomics approaches. To monitor in parallel hundreds or even thousands of metabolites, high-throughput techniques are required that enable screening for relative changes rather than absolute concentrations of compounds. Most analytical techniques for profiling small molecules consist of gas chromatography (GC) or high-performance liquid chromatography (HPLC) coupled to mass spectrometry. HPLC separations are better suited for the analysis of labile and high molecular weight compounds, and for the analysis of nonvolatile polar compounds in their natural form. Although GC- and HPLC-based profiling techniques are not truly quantitative, the compounds detecting and employing the acceptable standards may compare their relative amounts. We have demonstrated that reversed-phase monolithic capillary chromatography and hydrophilic chromatography can be successfully applied for sufficient plant crude extracts separations and metabolomics studies.

Arabidopsis↗

Analysis of dexamethasone and betamethasone in bovine urine by purification with an "on-line" immunoaffinity chromatography-high-performance liquid chromatography system and determination by gas chromatography-mass spectrometry.

A method for the immunoaffinity extraction of dexamethasone and betamethasone in bovine urine, followed by high-pressure liquid chromatography (HPLC) fractionation and gas chromatography-mass spectrometry determination, is described. A commercial immunoaffinity gel, containing antibodies raised against dexamethasone, was used to prepare an immunoaffinity cartridge which was inserted in an automatic HPLC system for on-line extraction and purification. By injecting urine samples (spiked with flumethasone as internal standard) directly into the system, it was possible to collect purified fractions, containing the analytes of interest. The fractions were dried and derivatized to yield the tetra-trimethylsilyl derivatives of the three corticosteroids, which were analyzed by selected ion monitoring gas chromatography-mass spectrometry. The method allowed a very good purification of samples and reached a detection limit of 0.1 ng/ml for dexamethasone and 0.2 ng/ml for betamethasone. Several samples, coming from a steer treated with dexamethasone and from other bovines coming from breedings in northern Italy, were analyzed with the method described. Dexamethasone levels ranged from 0.12 to 146 ng/ml.

Animals↗

Packed column chromatography, high-resolution gas-chromatography and high pressure liquid chromatography in comparison for the analysis of cannabis constituents.

The identification and the quantitative estimation of cannabis constituents is important for forensic purposes. High resolution gas-chromatography gives better results than gas-liquid chromatography with packed columns, as it shows a better resolution and higher number of constituents. Different quantitative values were found with the two chromatographic procedures. High-pressure liquid chromatography revealed the presence of cannabinoid acids in fresh cut influorescences of cannabis plants. The ratio acid/neutral cannabinoid may be useful in supplying information about the age of the cannabis preparations.

Cannabidiol↗

Validation study on 660 pesticide residues in animal tissues by gel permeation chromatography cleanup/gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry.

A new method using gel permeation chromatography (GPC) cleanup followed by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS) has been established for quantitative determination of 437 pesticide residues in animal tissues such as beef, mutton, pork, chicken, and rabbit. Based on an appraisal of the characteristics of both GC-MS and LC-MS-MS, validation experiments were conducted for 660 pesticides. In the method, 10 g animal samples were mixed with 20 g sodium sulfate and extracted with 35 mL of cyclohexane+ethyl acetate (1+1) twice by blender homogenization, centrifugation, and filtration. Evaporation was conducted and an equivalent of 5 g sample was injected into a 400 mm x 25 mm S-X3 GPC column, with cyclohexane+ethyl acetate (1+1) as the mobile phase at a flow rate of 5 mL/min. The 22-40 min fraction was collected for subsequent analysis. For the 368 pesticides determined by GC-MS, the portions collected from GPC were concentrated to 0.5 mL and exchanged with 5 mL hexane twice. For the 69 pesticides by LC-MS-MS, the portions collected from GPC were dissolved with acetonitrile+water (60+40) after taking the extract to dryness with nitrogen gas. In the linear range of each pesticide, the correlation coefficient was r > or = 0.98, exceptions being dinobuton, linuron, and fenamiphos sulfoxide. At the low, medium and high three fortification levels of 0.2-4800 microg/kg, recoveries fell within 40-120%, among which 417 pesticides recoveries between 60% and 120%, accounting for 95%, 20 analytes between 40% and 60%, accounting for 5%. The relative standard deviation was below 28% for all 437 pesticides. The limits of detection for the method were 0.2-600 microg/kg, depending on each pesticide.

Animals↗

Identification of triacylglycerols by high-performance liquid chromatography-gas-liquid chromatography and liquid chromatography-mass spectrometry.

Triacylglycerols from rat adipose tissue were chromatographed by high-performance liquid chromatography (HPLC), with a gradient of propan-2-ol in acetonitrile as the mobile phase. Fractions of the material eluting from the column were collected and analysed by automated gas - liquid chromatography of the fatty acid methyl esters obtained after transmethylation. Triacylglycerols were identified by using a combination of their fatty acid content and elution time from the HPLC column. Fractions corresponding to whole peaks or groups of peaks were also collected and re-chromatographed on a liquid chromatography - mass spectrometry system equipped with a belt interface. For most triacylglycerols, good agreement was obtained between the two methods, although mass spectrometric identification of the early eluting peaks was complicated by poor resolution of the triacylglycerols on the HPLC system.

Adipose Tissue↗

Overview of methods for the determination of trans fatty acids by gas chromatography, silver-ion thin-layer chromatography, silver-ion liquid chromatography, and gas chromatography/mass spectrometry.

trans Isomers of naturally occurring cis-unsaturated fatty acids are produced when liquid vegetable oils or marine oils are partially hydrogenated to produce margarine, shortenings, and other hardened-fat products. Isomeric trans fatty acids are also formed in the intestinal tract of ruminants, and they appear in small amounts in dairy products and ruminant meat. Currently, satisfactory analyses for the fatty acid profiles of fats containing trans fatty acids are obtained by gas chromatography (GC) using capillary columns coated with highly polar cyanosilicone stationary phases. In capillary GC methods, the key limitation has been the incomplete separation of trans-monoenoic acid isomers from their cis isomers; however, recent reports have demonstrated that improvements in separation are attainable with the use of 100 m columns. In these columns, there is very little overlap of cis and trans isomers. More accurate trans fatty acid analyses can be obtained by coupling GC with either silver-nitrate thin-layer chromatography or silver-nitrate liquid chromatography.

Chromatography, Liquid↗

Methods for analysis of conjugated linoleic acids and trans-18:1 isomers in dairy fats by using a combination of gas chromatography, silver-ion thin-layer chromatography/gas chromatography, and silver-ion liquid chromatography.

Conjugated linoleic acids (CLA) are octadecadienoic acids (18:2) that have a conjugated double-bond system. Interest in these compounds has expanded since CLA were found to be associated with a number of physiological and pathological responses such as cancer, metastases, atherosclerosis, diabetes, immunity, and body fat/protein composition. The main sources of these conjugated fatty acids are dairy fats. Rumen bacteria convert polyunsaturated fatty acids, especially linoleic and linolenic acids, to CLA and numerous trans- containing mono- and diunsaturated fatty acids. It has been established that an additional route of CLA synthesis in ruminants and monogastric animals, including humans, occurs via delta9 desaturation of the trans-18:1 isomers. To date, a total of 6 positional CLA isomers have been found in dairy fats, each occurring in 4 geometric forms (cis,trans; trans,cis; cis,cis; and trans,trans) for a total of 24. All of these CLA isomers can be resolved only by a combination of gas chromatography (GC), using 100 m highly polar capillary columns, and silver-ion liquid chromatography, using 3 of these 25 cm columns in series. Complete analysis of all the trans-18:1 isomers requires prior isolation of trans monoenes by silver-ion thin-layer chromatography (TLC), followed by GC analysis using the same 100 m capillary columns operated at low temperatures starting from 120 degrees C. These analytical techniques are required to assess the purity of commercial CLA preparations, because their purity will affect the interpretation of any physiological and/or biochemical response obtained. Prior assessment of CLA preparations by TLC is also recommended to determine the presence of any other impurities. The availability of pure CLA isomers will permit the evaluation and analysis of individual CLA isomers for their nutritional and biological activity in model systems, animals, and humans. These techniques are also essential to evaluate dairy fats for their content of specific CLA isomers and to help design experimental diets to increase the level of the desired CLA isomers in dairy fats. These improved techniques are further required to evaluate the CLA profile in monogastric animals fed commercial CLA preparations for CLA enrichment of animal products. This is particularly important because absorption and metabolism will alter the ingested-CLA profile in the animal fed.

Animals↗

Liquid chromatographic analysis of a potential polymeric-pendant drug delivery system for peptides. Application of high-performance size-exclusion chromatography, reversed-phase high-performance liquid chromatography and ion chromatography to the evaluation of biodegradable poly[(chloromethoxytrialanine methyl ester)phosphazenes].

A novel water-soluble polymer, poly[(chloromethoxytrialanine methyl ester)phosphazene] (poly-Tame), was characterized and evaluated using high-performance size-exclusion chromatography, gradient reversed-phase high-performance liquid chromatography and ion chromatography. These novel liquid chromatographic methods were validated for application to in vitro biodegradation experiments of poly-Tame in aqueous solutions. Results from method validation experiments are presented.

Biodegradation, Environmental↗

[Isolation, purification and identification of geniposidic acid in Eucommia ulmoides oliv. by silica column chromatography, reversed-phase high performance liquid chromatography, liquid chromatography-electrospray ionization mass spectrometry and nuclear magnetic resonance].

The methods using silica column chromatography, reversed-phase high performance liquid chromatography, liquid chromatography-electrospray ionization mass spectrometry and nuclear magnetic resonance (RP-HPLC/LC-ESI-MS/NMR) for the isolation, purification and identification of geniposidic acid (GPA) in Eucommia ulmoides Oliv. were established. The crude extract of E. ulmoides was obtained after E. ulmoides was extracted with 70% ethanol and the extract was concentrated under reduced pressures. The obtained crude extract dissolved in methanol was injected to a silica gel column and eluted with chloroform-methanol. The eluted fractions were analyzed by RP-HPLC. The eluant from chloroform-methanol (8:1, v/v) was indicated to be a single component by HPLC with a retention time of 5.142 min. The HPLC analysis of the mixture of this fraction with a GPA standard resulted in a single peak. The ultraviolet and infrared spectra of the eluted solution were essentially the same to those of GPA. On the other hand, LC-ESI-MS, 1H- and 13C-NMR experiments also indicated that the fraction was identical to GPA.

Chromatography, High Pressure Liquid↗

Advances in chromatography for clinical drug analysis: supercritical fluid chromatography, capillary electrophoresis, and selected high-performance liquid chromatography techniques.

Advances have been made in chromatography complement immunoassay for clinical drug analysis. Chromatographic theory shows that the minimum detectable mass is directly proportional to the square of column radius. Small internal diameter columns are capable of analyzing lower analyte concentrations, and high resolution is achievable in open capillary columns, concomitant with greatly reduced mobile phase consumption and waste. This review, based on the author's experience and literature, focuses on supercritical fluid chromatography (SFC), capillary electrophoresis (CE), and selected high-performance liquid chromatography (HPLC) methodologies--microbore and direct-sample analysis (DSA) using commercially available Restricted Access Media (RAM) and REMEDi. In investigating the feasibility of SFC, the "normal-phase-like" selectivity of carbon dioxide was established, affecting the design of the extraction protocol and the elution order of drugs and metabolites. For example, the "more polar" tautomer eluted after FK-506, opposite to the order in the reversed-phase HPLC analysis. CE was investigated by Shihabi et al. for the analysis of pentobarbital and iohexol, while Evenson and Wiktorowicz performed preliminary evaluation of several therapeutic drug monitoring (TDM) drug groups. Innovation in HPLC column technology and hardware have greatly enhanced clinical drug analysis. Microbore column, offering enhanced mass sensitivity and high resolution, utilizes small sample size of 5 microliters of serum for the analysis of chloramphenicol. Commercially available RAM include internal surface reversed phase, shielded hydrophobic phase, and dual zone media, readily applicable for serum drug analysis without any sample preparation. Recently, an automated HPLC REMEDi offers urine and serum drug screening for toxicology.

Animals↗