Search results for "Elution"
showing 10 items of 337 documents
Resolution of mixtures of steroidal hormones with micellar eluents of sodium dodecyl sulphate and acetonitrile or pentanol
2000
An optimization strategy was applied to explore the capability of hybrid micellar eluents of sodium dodecyl sulphate (SDS), using acetonitrile or pentanol as modifiers, to resolve mixtures of eleven steroids showing a wide range of hydrophobicity (clostebol acetate, dehydrotestosterone, dydrogesterone, medroxyprogesterone, medroxyprogesterone acetate, methandienone, methyltestosterone, progesterone, testosterone, testosterone enanthate and testosterone propionate). The accurate prediction of the retention behaviour of the steroids, with relative errors in the 0.8–1.7% and 0.4–2.9% ranges for SDS-acetonitrile and SDS-pentanol eluents, respectively, demonstrated the reliability of the methodo…
DETERMINATION OF STEROIDAL HORMONES IN URINE SAMPLES BY MICELLAR LIQUID CHROMATOGRAPHY FOLLOWING SOLID-PHASE EXTRACTION
2001
Steroidal hormones were determined in spiked urine samples using micellar mobile phases of sodium dodecyl sulphate (SDS)-pentanol, solid-phase extraction (SPE), and detection in the UV region. In the optimized procedure, a 10 mL aliquot of urine sample is loaded into a C18 cartridge and washed with 2 mL of 50:50 (v/v) methanol-water, followed by 200 μL of 70:30 (v/v) methanol-water. The retained steroids are eluted with 2 mL of methanol and the eluate evaporated to dryness under nitrogen at 50°C. The residue is redissolved with 200 μL of the micellar mobile phase used in the chromatographic separation and injected into the chromatograph. The performance of the procedure was checked for 13 s…
On-line determination of bipyridylium herbicides in water by HPLC
1997
Selective on-line solid phase extraction (SPE) and liquid chromatography determination (HPLC) of diquat, paraquat and difenzoquat from environmental water samples has been accomplished with Graphitized Carbon Black (GCB) as both extraction and analytical columns. The method involved passing of 50 mL of water through a cartridge filled with Carbograph. In the elution step, the herbicides were transferred from the cartridge to the analytical column (Hypercarb) by mean of a gradient of pH 3 aqueous solution of tetramethylammonium hydroxide (TMAOH) and ammonium sulphate and methanol. Hypercarb columns were found to give a low probability of false positives for bypiridylium herbicides and are ve…
Screening of some banned aromatic amines in textile products from Indian bandhani and gamthi fabric and in human sweat using micellar liquid chromato…
2021
Certain dyes in textile products, which are capable of reductively splitting into carcinogenic aromatic amines, are strictly controlled in many countries. A simple, rapid, sensitive and green chromatographic method has been developed and validated for the simultaneous determination of 4-aminophenol (4-AMP), p-phenylenediamine (p-PPD) and benzidine (BNZ), banned aromatic amines in dyeing clothes and human sweat. The separation was achieved using a micellar mobile phase of 0.1 M SDS, 4% 1- butanol (v/v) buffered to pH 7 with sodium dihydrogen phosphate, flowing under isocratic mode at 1 mL/min through a C18 column. Photodiode array detector was set at 210 nm. Using the above chromatographic c…
Benefits of solvent concentration pulses in retention time modelling of liquid chromatography
2019
The advantages and disadvantages of the use of isocratic experimental designs including transient increments of organic solvent (i.e., pulses) in the mobile phase(s) of lowest elution strength are explored with modelling purposes. For retained solutes, this type of mixed design offers similar or better predictive capability than gradient designs, shorter measurement time than pure isocratic designs, and retention model parameters that agree with those derived from pure isocratic experiments, with similar uncertainties. The predicted retention times are comparable to those offered by models adjusted from pure isocratic designs, and the solvent waste is appreciably lower. Under a practical st…
Stability of irinotecan-loaded drug eluting beads (DC BeadTM) used for transarterial chemoembolization
2009
Purpose. The aim of this study was to determine the loading efficiency, physicochemical stability, and release of irinotecan-loaded DC BeadsTM (bead size 100—300 μm, 300—500 μm) before and after mixing with nonionic contrast medium (Accupaque® 300, Imeron® 300, Ultravist ® 300) during a prolonged period of time (28 days) when stored at room temperature or refrigerated. Methods. DC Beads TM were loaded with 50 mg irinotecan (Campto®) per milliliter beads in a 2 h loading period. Drug loading efficiency and stability were determined by measuring the irinotecan concentration in the excess solution. A free-flowing in vitro elution method for a period of 2 h and phosphate buffered solution (PBS…
Global retention models and their application to the prediction of chromatographic fingerprints
2020
Abstract The resolution of samples containing unknown compounds of different nature, or without standards available, as is the case of chromatographic fingerprints, is still a challenge. Possibly, the most problematic aspect that prevents systematic method development is finding models that describe without bias the retention behaviour of the compounds in the samples. In this work, the use of global models (able to describe the whole sample) is proposed as an alternative to the use of individual models for each solute. Global models contain parameters that are specific for each solute, while other parameters ‒related to the column and solvent‒ are common for all solutes. A special regressio…
Estimation of significant solvent concentration ranges and its application to the enhancement of the accuracy of gradient predictions.
2004
Abstract The solvent concentration range actually useful for gradient predictions is significantly narrower than the total range scanned in a gradient run. This range, called “solvent informative range” (SIR), if known with the highest accuracy, allows to predict gradient retention times ( t g ) with minimal error. The small size of the SIR supports the application of the linear solvent strength theory (LSST). Furthermore, LSST allows a closed-form solution to the integral required to predict gradient retention times, which eliminates numerical integration, needed with other retention models. A methodology that calculates the SIR by applying error analysis, and uses it to improve the accura…
Preparation of electrophoretic variants of Corticosteroid-binding Globulin (CBG) using liquid liquid partition chromatography
1988
Abstract Human corticosteroid-binding globulin (CBG) was purified to homogeneity by application of three different chromatographic methods. After fractionation of pregnancy serum with ammonium sulfate the 80%-pellet was used for affinity chromatography based on tresyl activated Sepharose (Pharmacia, Uppsala, Sweden). The affinity eluate was injected into a Mono Q anion exchange column (Pharmacia). Fractions containing CBG were finally purified by liquid liquid chromatography on LiParGel 750 (Merck, Darmstadt, F.R.G.) 1,2 . The purified protein was characterized by IEF and PAGE. This paper describes a method for the chromatographic separation of the two variants of CBG without a loss of bind…
Study of the column efficiency using gradient elution based on Van Deemter plots.
2018
Performance of chromatographic columns is of major importance in the development of more efficient separation methods. So far, a common practice is to study the column behavior in isocratic elution by modifying the flow rate and fitting the theoretical plate height values versus the mobile phase linear velocity, according to the Van Deemter equation. In this work, an approach is presented to extend the measurement of efficiency to linear gradient elution, where the mean retention factor is kept constant at each assayed flow. This avoids a possible source of uncertainty due to the change in the distribution equilibria profile, and makes the mean interactions with the stationary phase in grad…