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PubMed1999

On-line solid-phase extraction and isocratic separation of retinoic acid isomers in microbore column switching system.

On-line solid-phase extraction coupled with micro-HPLC by column switching is an ideal technique for the analysis of retinoic acid in serum or plasma. The advantages are mainly contributed to an automated sample workup and low detection limits. On-line processing of the sample ensures minimal losses and full light protection during the entire procedure. Critical steps such as evaporation, extraction, and multiple transfers are avoided. Furthermore, the precision of highly automated methods is generally better than manual methods. We have successfully coupled a 2.1-mm I.D. analytical column with a 2.1-mm extraction column. This setup allows for large amounts of supernatant to be injected onto precolumns for concentration and cleanup. By means of column switching, this concentrate is transferred to the microcolumn with a highly reduced volume. The reduced diameter of the analytical column and the on-line solid-phase extraction allow for the fully automated quantification of as little as 100 fmol all-trans-retinoic acid in human serum. The detection limits obtained with these column switching techniques can compete with LC-MS. This new micro-HPLC method will be useful for the quantitation of endogenous retinoic acid metabolites, which are present at very low concentrations in biological material. Furthermore, more sensitive methods might also lead to the discovery of hitherto unknown retinoic acid metabolites. The combination of on-line SPE and micro-HPLC has, to our knowledge, not been used previously for retinoic acid analysis. The development of isocratic separation methods for retinoic acid isomers made this possible.

Chromatography, High Pressure Liquid↗
PubMed2001

LC determination of Z-338, novel gastroprokinetic agent in dog plasma by SCX solid phase extraction.

A simple high-performance liquid chromatographic assay with using UV detection (266 nm) was developed to determine a novel gastroprokinetic agent, Z-338 in dog plasma. The extraction procedure using solid-phase extraction with a Isolute SCX column produces extremely clean eluates and a high recovery. Intra- and inter-day variabilities were lower than 5%. The limit of quantitation of the method was 2.5 ng/ml. This assay was applied to the monitoring of Z-338 concentrations in dogs after oral administration. The method also appeared rapid, simple and suitable for therapeutic Z-338 monitoring.

Animals↗
PubMed1995

Solid-phase extraction of nicotine and its metabolites for high-performance liquid chromatographic determination in urine.

A solid-phase extraction, using Extrelut-1 glass columns, has been applied to urine samples of both passive and active smokers for high-performance liquid chromatographic determination of nicotine and its metabolites cotinine and trans-3'-hydroxycotinine. Chromatography was performed using a reversed-phase LC8DB column and a mobile phase consisting of water-acetonitrile (80:9, v/v) containing 5 ml triethylamine, 670 mg/l sodium heptanesulphonate, and 0.034 M each of K2HPO4 and citric acid (pH 4.4), at a flow-rate of 1.6 ml/min. The results obtained indicate that solid-phase extraction is a reliable and quick procedure which can be applied also to other nicotine metabolites.

Chromatography, High Pressure Liquid↗
PubMed2004

A high-throughput and sensitive methodology for the quantification of urinary 8-hydroxy-2'-deoxyguanosine: measurement with gas chromatography-mass spectrometry after single solid-phase extraction.

8-hydroxy-2'-deoxyguanosine (8OHdG) is a widely used biomarker for the measurement of endogenous oxidative DNA damage. A sensitive method for the quantification of 8OHdG in urine by single solid-phase extraction and GC-MS (gas chromatography with MS detection) using selective ion monitoring is described in the present study. After solid-phase extraction, samples are freeze-dried, derivatized by trimethylsilylation and analysed by GC-MS. The urinary 8OHdG was quantified using heavy isotope dilution with [18O]8OHdG. The recovery of 8OHdG after the solid-phase extraction ranged from 70 to 80% for a wide range of urinary 8OHdG levels. Using 1 ml of urine, the limit of quantification was >2.5 nM (2.5 pmol/ml) and the calibration curve was linear in the range 2.5-200 nM. This method was applied to measure 8OHdG in urine samples from 12 healthy subjects. The intra- and inter-day variations were <9%. Urinary 8OHdG levels in spot urine samples from four healthy subjects were also measured for 1 week and, again, the variation was small. The presence of H2O2 in urine did not cause artifactual formation of 8OHdG. Since this assay is simple, rapid, sensitive and reproducible, it seems suitable to be used as a routine methodology for the measurement of urinary excretion of 8OHdG in large population studies.

8-Hydroxy-2'-Deoxyguanosine↗
PubMed2001

Bioequivalence evaluation of two brands of cefaclor 500 mg capsules: quantification of cefaclor using solid phase extraction technique.

OBJECTIVE: To assess the bioequivalence of two cefaclor 500 mg capsule formulations, and to develop a new high performance liquid chromatographic (HPLC) method using solid phase extraction technique for the quantification of cefaclor in human plasma. METHOD: An open, randomized, two-way, crossover trial with a one-week washout period in 25 healthy volunteers. The two commercial brands used were Recocef(Julphar, United Arab Emirates) as test and Ceclor(Eli Lilly, UK) as reference product. The drug was administered with 240 mL of water after a 10-h overnight fast. After dosing, serial blood samples were collected for a period of 8 h. Plasma harvested from blood was analysed for cefaclor by a new HPLC method using a solid phase extraction technique. The limit of detection of cefaclor was 17.6 ng/mL; average recovery was 96.5%; the intraday CV was less than 8% and interday CV was less than 13%. Various pharmacokinetic parameters, including AUC0-t, AUC0-infinity, Cmax, Tmax, T1/2, and Kel, were determined from plasma concentrations for both formulations. Statistical analysis (ANOVA and 90% confidence intervals) were applied to AUC0-t, AUC0-infinity and Cmax for bioequivalence evaluation of two brands. The new HPLC method with solid phase extraction circumvented the problem of mixed polarity of cefaclor and facilitated its extraction from the complex plasma matrix while keeping the background free from interference due to endogenous plasma compounds. RESULTS: No significant difference was observed between the two brands of cefaclor capsules. CONCLUSION: Recocef was judged bioequivalent to Ceclor and the two products can therefore be considered to be interchangeable in medical practice.

Adolescent↗
PubMed2006

Multiwalled carbon nanotubes as sorbent for on-line coupling of solid-phase extraction to high-performance liquid chromatography for simultaneous determination of 10 sulfonamides in eggs and pork.

The sulfonamides (SAs) have been widely used as effective chemotherapeutics and growth promoters in animals' feeding, but their residues could be a potential danger to human health due to their carcinogenic potency and possible antibiotic resistance. Development of a simple and sensitive method for the determination of SAs residues in food of animal origin, therefore, is of great significance. An on-line solid-phase extraction (SPE) method using multiwalled carbon nanotubes as sorbent coupled with high-performance liquid chromatography (HPLC) for simultaneous determination of 10 sulfonamides (SAs) in eggs and pork was developed. The adsorptive potential of carbon nanotubes for solid-phase extraction of sulfonamides was investigated for the first time in the present paper. To on-line interface solid-phase extraction with HPLC, a conventional sample loop on the six-port injector valve of the HPLC was replaced by a preconcentration column packed with carbon nanotubes. The analytes in water solution were preconcentrated onto the preconcentration column and subsequently eluted with mobile phase of methanol-water (22:78). The developed on-line solid-phase extraction method for HPLC permitted the current HPLC separation and the next preconcentration proceeded in parallel, and thus allows one determination finished within 35 min. The RSD of 10 SAs for nine replicate measurements of a standard mixture of 1 microgl(-1) were in the range of 2.5-7.8%. The method was applied to the determination of trace sulfadiazin (SDZ), sulfamerazine (SMR), sulfadimidine (SDMD), sulfathiazole (STZ), sulfamoxol (SMO), sulfamethizole (SMT), sulfamethoxypyridazine (SMP), sulfachlorpyridazine (SCP), sulfadoxin (SDX) and sulfisoxazole (SIA) in eggs and pork. The results indicated that the proposed method was simple, cost-effective and sensitive.

Animals↗
PubMed2000

Immunoaffinity solid-phase extraction for the trace-analysis of low-molecular-mass analytes in complex sample matrices.

Immunoaffinity solid-phase extraction (SPE) sorbents, so-called immunosorbents (ISs), are based upon molecular recognition using antibodies. Thanks to the high affinity and high selectivity of the antigen-antibody interaction, they allow a high degree of molecular selectivity and have shown to be a unique tool in the sample preparation area these last few years. Extraction and clean-up of complex biological and environmental aqueous samples are achieved in the same step and from large volumes when required. Their application to extracts from solid matrixes is solvent-free and more simple than any other clean-up procedure. Single analytes can be targeted, but since an antibody can also bind one or more analytes having structure similar to the one used for its preparation, ISs have been developed for targeting a single analyte and its metabolites. The cross-reactivity was also exploited for developing ISs that could selectively extract a whole class of structurally related compounds. This review describes the current technology used for the synthesis of the ISs, their properties and their field of application. The different parameters governing the antigen-antibody interactions and the solid-phase extraction process are discussed. Emphasis is given to the optimisation of the SPE sequence, especially to the desorption and regeneration steps. The importance of the capacity and its relationship with the analytes recovery and breakthrough volumes is highlighted for class-specific ISs. Multi-class-selective ISs are also presented. Validation studies are reviewed using various certified reference materials. Relevant examples, involving combination with chromatography in both off-line and on-line mode, illustrate the high selectivity provided in various complex matrixes. Miniaturisation is also described, since it allows high throughput of samples.

Animals↗
PubMedDate not supplied

Effective one/two step purification of various materials by solid-phase extraction.

Simple one/two step purification procedures based on the solid-phase extraction technique were effectively exploited to clean up radiolabelled drugs represented by dihydrochloride of [6-3H]-stobadine and hydrochloride of [4-3H]-pentacaine, derivatization agents such as 4-nitrobenzoyl chloride or 3,5-dinitrobenzoyl chloride, as well as the aqueous phosphate or triethylamine acetate buffer solutions.

Carbamates↗
PubMed1998

On-line dialysis solid-phase extraction coupled to capillary electrophoresis.

A fully automated dialysis solid-phase extraction (SPE) sample preparation procedure is coupled on-line to capillary electrophoresis (CE) for the first time. The system is used to determine sulfonamides in serum and urine. The dialysis unit serves to remove proteins and particulate matter. Reconcentration of the analytes is performed with a small SPE column while (in)organic salts and other interferences are removed simultaneously. Finally, the analytes are desorbed and injected, via a homemade interface, into the CE system. Limits of detection (LOD) of 0.05-0.1 and 0.05-0.3 microg/mL are obtained in urine and serum, respectively. The within-day and between-day precisions are in the range of 2-6% and 3-8%, respectively, for a concentration of five times the LOD. The dialysis SPE-CE system was used over a period of six months for the analysis of over 500 serum and urine samples without problems such as clogging of the CE capillary or SPE column.

Body Fluids↗
PubMed2006

Determination of M+4 stable isotope labeled cortisone and cortisol in human plasma by microElution solid-phase extraction and liquid chromatography/tandem mass spectrometry.

A sensitive microElution solid-phase extraction (SPE) liquid chromatography/tandem mass spectrometry (LC/MS/MS) method has been developed and validated for the determination of M+4 stable isotope labeled cortisone and cortisol in human plasma. In this method, M+4 cortisone and M+4 cortisol were extracted from 0.3 mL of human plasma samples using a Waters Oasis HLB 96-well microElution SPE plate using 70 microL methanol as the elution solvent, and chromatographed on a Waters Symmetry C18 column (4.6 x 50 mm, 3.5 microm). M+9 cortisone and M+9 cortisol were used as the internal standards. A PE Sciex API 4000 tandem mass spectrometer interfaced with the liquid chromatograph via a turboionspray source was used for mass analysis and detection. The selected reaction monitoring (SRM) of precursor --> product ion transitions were monitored at m/z 365.2 [M+H](+) --> 167.0 and at m/z 367.3 [M+H](+) --> 125.1 for M+4 cortisone and M+4 cortisol, respectively. The lower limit of quantitation was 0.1 ng mL(-1) and the linear calibration range was from 0.1 to 100 ng mL(-1) for both analytes. This method demonstrated to be very reproducible and reliable.

Blood Chemical Analysis↗
PubMed2000

Analysis of multiple pesticides in urban storm water using solid-phase extraction.

An analytical method was developed using C(18) solid-phase extraction and gas chromatography-nitrogen phosphorus detection (GC-NPD) to determine the presence and quantity of 12 contemporary pesticides in storm water runoff from an urban environment. The method was validated, using deionized water and water collected from a local pond, for two concentration levels and four holding time regimes. The method was then utilized in a study examining nonpoint source (NPS) pollution in Wichita, KS. Accuracy and precision were demonstrated in each test for each analyte except diazinon, which degraded rapidly during holding times in aqueous solution. For all matrices, concentration levels, and holding times, mean recoveries for the remaining 11 pesticides ranged from 50% to 105% with percent relative standard deviations less than 25%.

Chromatography, Gas↗
PubMedDate not supplied

Solid-phase extraction of 1,4-benzodiazepines from biological fluids.

The solid-phase extraction (SPE) of seven 1,4-benzodiazepines (oxazepam, diazepam, temazepam, nordazepam, brotizolam, adinazolam and midazolam) using prazepam as internal standard was investigated. The 1,4-benzodiazepines were recovered from an aqueous buffer of suitable pH, using C18 Sep-Pak cartridges and mixtures of methanol-water as elution solvent. The recovery of oxazepam using different sorbent materials (C2, C8, C18, cyanopropyl, phenyl and cyclohexyl Bond-Elut) was also examined as a function of pH and the composition of the elution solvent. The SPE of oxazepam was investigated using spiked urine samples and the C2 cartridge gave rise to the cleanest urine extracts. The recoveries of the other 1,4-benzodiazepines from spiked urine and plasma samples using the C2 cartridge was then found to be higher than 90%, without any interference from endogenous compounds of the samples. Finally, the influence of other factors such as drug concentration, sample volume and the number of times the SPE cartridge had been used was also examined.

Benzodiazepines↗
PubMed2005

Molecularly imprinted solid-phase extraction of (-)-ephedrine from Chinese Ephedra.

Method of molecularly imprinted solid phase extraction (MISPE) of (-)-ephedrine from Chinese Ephedra has been developed in the research. The molecularly imprinted polymer (MIP) with good selectivity and affinity for (-)-ephedrine was synthesized with (-)-ephedrine as the template, methacrylic acid as the functional monomer. The washing and elution conditions in MISPE were selected and optimized for efficient analyte extraction and sample clean-up. A clean analytical HPLC base line of ephedra extract was obtained after MISPE, which indicated that the sample pre-treatment was efficient. Good recovery and precision were obtained in the assessment for the MISPE-HPLC procedure, which demonstrated it is a reliable method and can be used for the determination of (-)-ephedrine in herbal ephedra.

Chromatography, High Pressure Liquid↗
PubMed2004

Bioanalysis of tobramycin for therapeutic drug monitoring by solid-phase extraction and capillary zone electrophoresis.

A method based on solid-phase extraction (SPE) and capillary zone electrophoresis (CZE) for the analysis of tobramycin in human serum is presented. An off-line SPE employing a carboxypropyl bonded phase (CBA) cartridge was used for the extraction of tobramycin from human serum. Adsorbed tobramycin was eluted from the CBA cartridge using a mixture of NH(3) (25%, w/v)-methanol (30:70, v/v). After evaporation, the analyte was reconstituted and derivatized with o-phthaldialdehyde (OPA)/3-mercaptopropionic acid (MPA). The resulting tobramycin-OPA/MPA derivative was purified, and then identified by mass spectrometry. The tobramycin-OPA/MPA derivative was then analysed by CZE with a background electrolyte (BGE) comprising of 30 mM sodium tetraborate pH 10.0-acetonitrile (ACN) (80:20, v/v) with ultraviolet detection at 230 nm. A linear response was observed in the range of 0.3-30 microg/ml with r(2) = 0.992. The sensitivity of the method was determined by its limit of quantitation (LOQ) and limit of detection (LOD) of 0.3 microg/ml and 0.1 microg/ml, respectively. SPE recovery ranged from 68 to 79% at the trough levels to 98% at the peak levels found in serum. Furosemide has been added as internal standard (IS) to improve precision. For the therapeutic range of tobramycin in serum (2-10 microg/ml) the relative standard deviation (R.S.D.) was less than 11% for the entire SPE/CE process. The method demonstrated excellent selectivity as shown by the lack of interference from a total of 20 drugs investigated. The method was then used in therapeutic drug monitoring of patients receiving the drug.

Anti-Bacterial Agents↗
PubMed2006

Quantification of antihistamine acrivastine in plasma by solid-phase extraction and high-performance liquid chromatography.

An automated solid-phase extraction method was developed for the determination of the H1-antihistamine acrivastine in plasma samples. Acrivastine was analyzed at the wavelength of 254 nm using a reversed-phase HPLC assay. Both extraction procedure and analytical condition were optimized and validated for maximum recovery and resolution. The developed method was further applied to plasma samples collected from an in vivo pharmacokinetic study in rabbits. The assay was found to be simple, specific, accurate and reproducible.

Animals↗
PubMed1999

Automated solid-phase extraction workstations combined with quantitative bioanalytical LC/MS.

An automated solid-phase extraction workstation was used to develop, characterize and validate an LC/MS/MS method for quantifying a novel lipid-regulating drug in dog plasma. Method development was facilitated by workstation functions that allowed wash solvents of varying organic composition to be mixed and tested automatically. Precision estimates for this approach were within 9.8% relative standard deviation (RSD) across the calibration range. Accuracy for replicate determinations of quality controls was between -7.2 and +6.2% relative error (RE) over 5-1,000 ng/ml(-1). Recoveries were evaluated for a wide variety of wash solvents, elution solvents and sorbents. Optimized recoveries were generally > 95%. A sample throughput benchmark for the method was approximately equal 8 min per sample. Because of parallel sample processing, 100 samples were extracted in less than 120 min. The approach has proven useful for use with LC/MS/MS, using a multiple reaction monitoring (MRM) approach.

Animals↗
PubMed2002

Solid-phase extraction procedure to remove organic acids from honey.

A solid-phase extraction procedure was applied to remove organic acids from honey. Malic, maleic, citric, succinic and fumaric acids were isolated with an anion-exchange cartridge. The different parameters which affected the extraction procedure were studied and optimised to establish the optimal conditions for maximum recovery of organic acids and minimum extraction of interferences. The optimised procedure used a cartridge which was activated with 10 ml of 0.1 M sodium hydroxide solution (percolation rate 3 ml/min). A 10 ml volume of honey solution was passed at a flow-rate of 0.5 ml/min. The cartridge was washed with 10 ml of water (3 ml/min) and organic acids were eluted with 4 ml of 0.1 M sulfuric acid (0.5 ml/min). This solution was injected directly into the chromatograph. When this procedure was carried out on standard solutions of organic acids, recoveries between 99.2 and 103.4% were found. If this procedure was applied to honey samples these recoveries were also satisfactory and ranged from 62.9 to 99.4%.

Acids↗
PubMed2001

Determination of aliphatic amines in water by liquid chromatography using solid-phase extraction cartridges for preconcentration and derivatization.

Bond Elut C18 solid-phase extraction cartridges were used for preconcentration and pre-column derivatization with 3,5-dinitrobenzoyl chloride (DNB) of aliphatic amines in water. Conditions for analyte preconcentration and derivatization (including the volume of sample, concentration of reagent, time of reaction and pH) were investigated, using ethylamine, isopropylamine and dimethylamine as model compounds. On the basis of these studies, a rapid and sensitive method for the determination of aliphatic amines in water is presented. The analytes are retained and purified on the cartridges and then derivatized and desorbed by drawing in succession the DNB solution and acetonitrile. The collected extracts are subsequently chromatographed in a Hypersil ODS C18 column using acetonitrile-water for elution. The DNB derivatives are monitored at 230 nm. The method provides satisfactory reproducibility and linearity within the 0.050-1.0 mg l(-1) concentration interval, the limits of detection being 2-5 microg l(-1). Analyte recoveries were in the 70-102% range, whereas the conversion yields compared with those observed for the solution derivatization were in the 79-107% range. The total analysis time (sample treatment plus chromatography) was about 15 min. The method was applied to the determination of ethylamine, isopropylamine and dimethylamine in tap and river waters.

Amines↗