Search results for " Phase"
showing 10 items of 1862 documents
On-line preconcentration strategies for analyzing pesticides in fruits and vegetables by micellar electrokinetic chromatography.
2007
Five pesticides (fludioxonil, procymidone, pyriproxyfen, dinoseb and carbendazim) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 20 mmol l(-1) phosphate buffer at pH 2.3, containing 25 mmol l(-1) sodium dodecylsulfate and 10% methanol. Three on-line concentration strategies, sweeping (SW), normal stacking with reversed migration and a water plug (SRW) and stacking with reverse migration and removal of sample matrix using polarity switching (SRMM), were compared. About 10-, 30- and 50-fold increases in detection sensitivity, compared with standard hydrodynamic injection (5 s at 0.5 psi), were observed with SW, SRW and SRMM, respectively. Limits of…
Improved Solid Phase Extraction Procedure for Assay of Cephalosporins in Human Urine Samples
1998
Abstract Solid phase extraction technique has been evaluated for the treatment of urine samples in the analysis of cephalosporins before injection into an HP-Hypersil ODS-C18 column. Cephalexin, cefotaxime, cefazolin, cefuroxime, and cefoxitin were tested with seven different reversed-phase extraction column cartridges and the obtained urine extracts were not clean. However, 3M Empore extraction disk cartridges packed with octadecyl (C18) bonded silica provided clean extracts with a single extraction. The recoveries of the five cephalosporins ranged from 56 to 60 % in the 1.25–500 g/mL concentration range. The assay was accurate, precise, and adequate for testing the drug content in urine s…
Effect of the shampoo Ultra Clean on drug concentrations in human hair
2000
The influence of the special shampoo Ultra Clean (Zydot Unlimited, Tulsa, Oklahoma) on the results of hair analyses was investigated. Hair samples from persons (n = 14) with a known history of drug abuse were collected at autopsy. The hair samples were divided into separate strands which were analyzed both after washing with Ultra Clean and without treatment. Hair analyses were performed by methanol extraction under sonication, purification by solid phase extraction and GC/MS in SIM mode according to routine procedures for tetrahydrocannabinol (THC), cocaine, amphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), methylenedioxyethylamphetamine (MDE), heroin, 6-m…
On-line in-tube solid phase microextraction-capillary liquid chromatography method for monitoring degradation products of di-(2-ethylhexyl) phthalate…
2014
Abstract The main di-(2-ethylhexyl) phthalate (DEHP) degradation products, (2-ethylhexyl) phthalate (MEHP), diethyl phthalate (DEP) and dibutyl phthalate (DBP), have been tested. The proposed cost-effective method combines on-line, in-tube solid-phase micro extraction (IT-SPME) in in-valve configuration and capillary liquid chromatography with UV diode array detection (Cap-LC-DAD). Acidification of the samples at pH 3 improved markedly the estimation of MEHP. Aliquots of 4 mL of acidified water samples were directly processed. After sample loading, the analytes were desorbed with the mobile-phase and transferred to the monolithic capillary column. Satisfactory linearity and precision, absen…
A solid-phase extraction and size-exclusion liquid chromatographic method for polyethylene glycol 25 p-aminobenzoic acid determination in urine: Vali…
2007
No previous publications about percutaneous absorption of polyethylene glycol 25 p-aminobenzoic acid (PEG-25 PABA) have been found in the literature and the expected levels to be found in human urine after sunscreens use are unknown. The method proposed here is suitable to determine PEG-25 PABA in the urine of sunscreens users in order to carry out studies on body accumulation/excretion. It is based on solid-phase extraction (SPE) with size-exclusion liquid chromatography determination. Solid-phase extraction allows the analyte to be retained and subsequently eluted for a clean-up, using a silica-based cartridge. The size-exclusion liquid chromatography of the eluted allows the rest of matr…
Determination of clenbuterol in urine by azo-dye precolumn derivatization and micellar liquid chromatography
1997
Clenbuterol has been determined in urine by solidphase extraction on a C18 cartridge, diazotization of the eluate with nitrite, coupling of the diazonium ion with 1-(naphthyl)ethylenediamine, and separation of the azo dye formed by HPLC with a C18 column and a micellar mobile phase containing 0.1 M sodium dodecyl sulphate, 12%n-butanol and 0.05 M citrate buffer, pH 3. Recoveries higher than 90% were obtained by mixing the samples with a 20% 0.2 M NaOH before extraction. Limits of detection of 51 and 6.7 ng L−1 were obtained with spectrophotometric and thermal lens spectrometric detection, respectively; respective repeatabilities were 3.1% (5 μg mL−1) and 5.6% (0.16 μg mL−1).
Simultaneous detection of three antiviral and four antibiotic compounds in source-separated urine with liquid chromatography
2013
An analytical method for the simultaneous screening of three antiviral agents (nevirapine, zidovudine, lamivudine), four antibiotics (sulfamethoxazole, trimethoprim, ciprofloxacin, rifampicin) and one reference compound (carbamazepine) in human urine was developed. Separation was achieved with a Kinetex XB-C18 (75 × 4.6 mm, 2.6 μm) column after the extraction of pharmaceuticals from urine with SPE. Gradient elution with a mobile phase consisting of acetonitrile and 10 mM KH2 PO4 (pH 2.5), and diode array detection with monitoring at 210 and 264 nm was applied. The developed method was validated in terms of selectivity, linearity, stability and sensitivity. Repeatability (n = 3) and between-…
Sensitive determination of probenecid in urine samples by reversed-phase liquid chromatography and UV-visible detection using solid-phase extraction …
1993
This study describes a rapid method for the determination of probenecid in human urine by liquid chromatography with UV detection at 254 nm, after clean-up through a C8 solid-phase extraction column. Liquid chromatography was carried out on a C18-bonded phase using an acetonitrile-acetate buffer (pH=4) gradient elution. Ethacrynic acid was used as internal standard. The system has been applied to the determination of probenecid in the 0.10–100.0 μg/ml concentration range; the limit of detection was 5 ng/mL.
Analysis of organic pollutants in water at trace levels using fully automated solid-phase extraction coupled to high-performance liquid chromatography
1997
A method has been developed for the determination of trace levels of 32 pesticides, 19 explosives and 16 polycyclic aromatic hydrocarbons (PAH) in water in three individual steps. Solid-phase enrichment (SPE) is coupled to high-performance liquid chromatography (HPLC) with a fully automated system. The organic pollutants are enriched on reusable cartridges packed with adsorbent materials: pesticides and explosives on a mixed bed of divinylbenzene-ethylvinylbenzene copolymers (LiChrolut EN®) and perfluorinated polyethylene (PolyF®), and polycyclic aromatic hydrocarbons on C18-modified silica (Zorbax® ODS1). Thermally assisted desorption (TAD) has been shown to increase the recovery of analyt…
Solid-phase extraction on C18 in the trace determination of selected polychlorinated biphenyls in milk.
1995
The utility of solid-phase extraction with octadecylsilica for determining fifteen polychlorinated biphenyl (PCB) congeners from milk samples was examined. Recoveries higher than 80% and relative standard deviations better than 10% were obtained for PCBs from different kinds of milk (whole, skimmed, 2%, powdered, breast and evaporated). A comparison with other procedures was made. The described method provides better detection limits than those attainable with the liquid-liquid extractions currently used as standard methods, when capillary gas-liquid chromatography is used for the final determination. A study of the separation was also performed using six different fused-silica capillary co…