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PubMed2006

Simultaneous determination of 6 beta-blockers, 3 calcium-channel antagonists, 4 angiotensin-II antagonists and 1 antiarrhythmic drug in post-mortem whole blood by automated solid phase extraction and liquid chromatography mass spectrometry. Method development and robustness testing by experimental design.

A method for the simultaneous determination of the beta-blockers atenolol, sotalol, metoprolol, bisoprolol, propranolol and carvedilol, the calcium-channel antagonists diltiazem, amlodipine and verapamil, the angiotensin-II antagonists losartan, irbesartan, valsartan and telmisartan, and the antiarrhythmic drug flecainide, in whole blood samples from forensic autopsies was developed. Sample clean-up was achieved by precipitation and solid phase extraction (SPE) with a mixed-mode column. Quantification was performed by reversed phase high performance liquid chromatography with positive electrospray ionization mass spectrometric detection (HPLC-MS). The method has been developed and robustness tested by systematically searching for satisfactory conditions using experimental designs including factorial and response surface designs. With the exception of amlodipine, the concentration limit of quantification (cLOQ) covered low therapeutic concentration levels for all the compounds. Within assay precisions and accuracies (bias) were 3.4-21% RSD and from -24 to 21% for the concentration range 1.00-5.00 microM, respectively. Between assay precisions were 4.4-28% RSD for the concentration range from 0.1 to 5 microM and recoveries varied from 9 to 103%. The method is used for determination of cardiovascular drugs in post-mortem whole blood samples from forensic autopsy cases.

Adrenergic beta-Antagonists↗
PubMed1999

Solid-phase extraction for the determination of caffeine in traditional Chinese medicinal prescriptions containing Theae folium by high performance liquid chromatography.

A high performance liquid chromatographic method in combination with C-18 reverse phase solid-phase extraction (SPE) was developed for determination of caffeine (CA) in traditional Chinese medicinal prescriptions which contain Theae folium. The frequently used prescriptions include Shin-Yi-San, Chuan-Chyong-Char-Tyau-San, Tsang-Eel-San, San-Hwang-Shyr-Gau-Tang, Tzy-Shenn-Ming-Mu-Tang and Shiang-Chyong-San. The present HPLC system uses a Merck RP-select B column by isocratic elution with methanol and 1% (v/v) acetic acid (1:4) as the mobile phase and detected at UV 270 nm. 8-Chlorotheophylline was used as an internal standard. The extracts of prescriptions were treated by Supelclean LC-18 SPE tube for eliminating interferences. Blank decoctions of each prescription were also examined as a test for interferences. The recoveries of caffeine from the Chinese medicinal prescriptions ranged from 88.5 to 92.3%. The relative standard deviations of caffeine ranged between 0.86 and 1.97% (intraday) and 1.04 and 3.90% (interday). The contents of caffeine in standard decoctions ranged from 13.98 to 19.62 mg g(-1).

Caffeine↗
PubMed1993

Solid phase extraction of trans-resveratrol from wines for HPLC analysis.

Some recent studies have put forward the hypothesis that the presence of trans-resveratrol (trans-3,5,4'-trihydroxystilbene) in red wine may be related to some of its therapeutic properties. A fundamental step in view of this evaluation is the development of a method for the quick, accurate and precise analysis of this compound. Sample enrichment and purification can be obtained by solid-phase extraction using reverse-phase C18 cartridges. HPLC analysis carried out by means of a photodiode-array detector, with an internal standard method, allows the detection of up to 10 micrograms/L in wine, with a linear range between 0.6 and 300 ng injected and a precision of 3.3%. The results of the first analyses show that the concentrations of trans-resveratrol in wines might be much higher than so far reported in the literature.

Cardiovascular Diseases↗
PubMed2001

A simple method for the assay of colistin in human plasma, using pre-column derivatization with 9-fluorenylmethyl chloroformate in solid-phase extraction cartridges and reversed-phase high-performance liquid chromatography.

A simple, selective and sensitive high-performance liquid chromatographic (HPLC) method is described for the determination of colistin in human plasma. Derivatization with 9-fluorenylmethyl chloroformate was performed in the same solid-phase extraction C18 cartridge used for sample pre-treatment, followed by reversed-phase HPLC with fluorimetric detection. Quantification was achieved using the ratio of the summed peak areas of colistin A and B derivatives to that of the derivative of netilmicin (internal standard). Linear calibration curves were obtained within the concentrations of colistin sulfate from 0.10 to 4.0 mg/l in plasma. Accuracy was within 10% and reproducibility (RSD) was less than 10%.

Calibration↗
PubMed2003

An amobarbital molecularly imprinted microsphere for selective solid-phase extraction of phenobarbital from human urine and medicines and their determination by high-performance liquid chromatography.

A 40-60 microm amobarbital molecularly imprinted microsphere, used as a solid-phase selective sorbent for extracting phenobarbital from human urine and medicines, was prepared by a suspension polymerization method. A series of binding studies was performed in order to find optimal loading, washing and eluting conditions for solid-phase extraction. Under optimal conditions, good recoveries of phenobarbital in samples were obtained. Normally, molecularly imprinted polymers, prepared in bulk, require laborious work. Significant losses occur during the procedure of grinding and washing. In this work all molecularly imprinted polymers made into microsphere could be utilized, and the cost of the template was reduced too (the price of phenobarbital is twice that of amobarbital). As the phenobarbital to be extracted was different from the template molecule amobarbital, the interference caused by template leaking could be avoided in the assay.

Amobarbital↗
PubMed1998

Solid-phase extraction procedures in systematic toxicological analysis.

In systematic toxicological analysis (STA) the substance(s) present is (are) not known at the start of the analysis. In such an undirected search the extraction procedure cannot be directed to a given substance but must be a general procedure where a compromise must be reached in that the substances of interest are isolated at a yield as high as possible and the interfering substances from the biological material are removed. When using solid-phase extraction (SPE) it is desirable to have procedures using just one column. An overview of screening procedures using diatomaceous earth, polystyrene-divinylbenzene copolymer and mixed-mode bonded silica as column material in SPE is given. The latter type of sorbent is most popular at the moment and the critical steps in the procedure are outlined in more detail. Recent developments of SPE disks look very promising for STA.

Adsorption↗
PubMed2003

Validated method for the simultaneous determination of Delta 9-tetrahydrocannabinol (THC), 11-hydroxy-THC and 11-nor-9-carboxy-THC in human plasma using solid phase extraction and gas chromatography-mass spectrometry with positive chemical ionization.

A fully validated, highly sensitive and specific method for the extraction and quantification of Delta(9)-tetrahydrocannabinol (THC), 11-hydroxy-Delta(9)-tetrahydrocannabinol (11-OH-THC) and 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THCCOOH) in plasma is presented. This method incorporates Escherichia coli beta-glucuronidase hydrolysis to cleave glucuronic acid moieties to capture total analyte concentrations, and simultaneous solid phase extraction (SPE) of the three analytes in a single eluant with separation and quantification on a bench-top positive chemical ionization (PCI) gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring (SIM) mode. Quantitation was achieved by the addition of deuterated analogues for each analyte as internal standards (IS). Limits of quantitation (LOQ) were 0.5, 0.5 and 1.0 for THC, 11-OH-THC and THCCOOH, respectively, with linearity ranging up to 50 ng/ml for THC and 11-OH-THC, and 100 ng/ml for THCCOOH. Absolute recoveries ranged from 67.3 to 83.5% for all three analytes. Intra-assay accuracy and precision ranged from 1.2 to 12.2 and 1.4 to 4.7%, respectively. Inter-assay accuracy and precision ranged from 1.4 to 12.2 and 3.1 to 7.3%, respectively. This method was used to analyze plasma samples collected from individuals participating in a controlled oral THC administration study. Statistically significant (P< or =0.05) increases of 40% for 11-OH-THC and 42% for THCCOOH concentrations were found between hydrolyzed and non-hydrolyzed results. This method will be utilized in ongoing controlled cannabinoid administration studies and may be a useful analytical procedure for the fields of forensic toxicology and cannabinoid pharmacology.

Dronabinol↗
PubMed2004

Effects of pH and competing anions on the speciation of arsenic in fixed ionic strength solutions by solid phase extraction cartridges.

Anion exchange resins (AERs) separate As(V) and As(III) in solution by retaining As(V) and allowing As(III) to pass through. Anion exchange resins offer several advantages including cost, portability, and ease of use. The use of AERs for the instantaneous speciation of As minimizes the effects of preservatives on As species analysis. The aims of this study were to: (1) Examine the effects of pH and competing anions on the efficacy of solid phase extraction cartridges (SPECs) for speciation of As in a 0.01 molL(-1) NaNO(3) background electrolyte. (2) Identify optimal conditions (e.g. flow rates) for As speciation. (3) Calculate method detection limits (MDLs) from spiked background electrolyte and percent recoveries of As species from spiked extracts of mine wastes. The most effective SPEC retained As(V) through a range of environmentally relevant pH values (4-8). The mass loading capacity for As(V) was reduced in the background electrolyte (0.006 mg) compared with As(V) in deionized H(2)O (0.75 mg). Some retention (10-20%) of As(III) occurred on pre-wetted cartridges. Approximately 98% of spiked As(III) passed through dry cartridges. The recommended flow rate (0.5 mL min(-1)) was increased to 5 mL min(-1) without significant effect on As(V) retention. The presence of anions decreased the retention of As(V) with sulfate and phosphate having the greatest impact. MDLs were 0.004 mg L(-1) for both inorganic species. Spike recoveries in 0.01 M NaNO(3) mine waste extracts averaged 94% for As(III) and 107% for As(V).

Anion Exchange Resins↗
PubMed1997

A tandem solid phase extraction, reversed-phase HPLC method for determining SDZ WAG 994 in dog, monkey and rat blood.

The development and validation of a sensitive and specific HPLC method for SDZ WAG 994 (I) in dog, monkey and rat blood is described. Sample preparation entailed double solid phase extraction (SPE) of I and the internal standard from 0.5 ml of animal blood using a phenyl and propyl sulfonic acid cation exchange column, sequentially. Chromatographic separation was achieved on a YMC Basic C-8 narrowbore HPLC column and the eluates were detected by UV absorption at 266 nm. The method has a linear response up to at least 1800 ng/ml with a limit of quantification of 1 ng/ml across all species. Analysis of 'blinded' quality control dog and monkey blood samples over 3 or 4 days produced median precisions of 2.89 and 4.77%, and median reproducibilities of 4.86 and 10.9%, respectively. Curve fitting of variability estimates indicated that concentration independent error contributed 3-9% of the total method error for the tandem SPE procedure. Extracted endogenous material from blood matrices, several potential metabolites and cyclohexyladenosine were well resolved from the peaks of interest. The stability of I in dog blood stored at -20 degrees C is at least 6 months. The overall absolute and relative recovery of I using the tandem SPE procedure was 85.5 +/- 5.1% and 96.5 +/- 5.0%, respectively. The ruggedness of the method has been demonstrated by multiple analyses, from several toxicokinetic studies, performed by different analysts using comparable instrumentation.

Adenosine↗
PubMed1997

A direct technique for the simultaneous determination of 10 drug candidates in plasma by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry interfaced to a Prospekt solid-phase extraction system.

New drug candidates are being synthesized at an ever increasing rate and, until recently, the pharmacokinetics of only a few of these could be evaluated. Our laboratory is taking a novel approach to rapid multiple pharmacokinetic screening of potential drug candidates in which mixtures of new substances are co-administered to animals and analyzed simultaneously in plasma using liquid chromatography with tandem MS/MS detection in conjunction with a Prospekt automated on-line solid-phase extraction system. Plasma is sampled via an autosampler and extracted by the Prospekt with the eluent being introduced directly via a reverse phase HPLC column and a heated nebulizer interface to the mass spectrometer. Generic extraction and chromatographic conditions generally give good recoveries. The chromatographic run-times are less than 8 min. The accuracy and precision of these assays are carefully controlled with recoveries generally in the range 80-120% and coefficients of variation less than 20%. Lower quantifiable limits range from 2.5 to 5 ng ml-1. This approach considerably reduces the number of animals needed to screen drug candidates and its power is illustrated by determination of the pharmacokinetics of 10 substances after their simultaneous administration to dogs.

Animals↗
PubMedDate not supplied

Determination of selamectin in dog plasma by high performance liquid chromatography with automated solid phase extraction and fluorescence detection.

A method is described for the determination of selamectin in dog plasma, using High-Performance Liquid Chromatography (HPLC) with fluorescence detection (excitation and emission wavelengths fixed at 355 and 465 nm, respectively). The fluorescent derivative was obtained by condensation reaction with trifluoroacetic anhydride and N-methylimidazole. The method employs 1 mL plasma samples and gives linear calibration graphs (r = 0.999) over the concentration range studied (0.5-50 ng mL(-1)). Automatic solid phase extraction using the benchmate procedure was used for sample preparation. This method permits the determination of selamectin at levels as low as 0.1 ng mL(-1) and its suitability was demonstrated by a pharmacokinetic study on a dog receiving the therapeutic dose (Spot-on administration).

Animals↗
PubMed2003

A comparative solid-phase extraction study for the simultaneous determination of fluoxetine, amitriptyline, nortriptyline, trimipramine, maprotiline, clomipramine, and trazodone in whole blood by capillary gas-liquid chromatography with nitrogen-phosphorus detection.

This paper reports the simultaneous detection of the seven antidepressants fluoxetine, amitriptyline, nortriptyline, trimipramine, maprotiline, clomipramine, and trazodone in whole blood at concentration levels of 100-2000 ng/mL by gas chromatography with a nitrogen-phosphorus detector (GC-NPD). A comparative and validation study using two solid-phase extraction (SPE) columns, Chem Elut and Bond Elut Certify, were developed regarding their recovery, precision, sensitivity, and matrix purification efficiency. The Chem Elut columns, a diatomaceous earth, are closely related to conventional liquid-liquid extraction. The Bond Elut Certify columns, more recently developed in the market, are a mixed SPE: reversed-phase and cation exchange sorbent. Recoveries of the compounds using Chem Elut columns at 500 ng/mL were in the range 30-50%, with intra- and interassay precisions of less than 9% and 17%, respectively. Limits of detection (LODs) and quantitation (LOQs) ranged from 13 to 146 ng/mL and from 44 to 485 ng/mL, respectively. Recoveries of the compounds using Bond Elut Certify columns at 500 ng/mL were in the range 59-84% with intra- and interassay precisions of less than 8% and 11%, respectively. LODs and LOQs ranged from 8 to 67 ng/mL and from 25 to 223 ng/mL, respectively. An excellent linearity was observed with both extraction procedures from the LOQs up to 2000 ng/mL. Higher recoveries, cleaner extracts, better sensitivity, better precision, and less solvent consumption and disposal were achieved for the screening of these antidepressants with the use of the mixed SPE Bond Elut Certify compared with Chem Elut columns.

Antidepressive Agents, Tricyclic↗
PubMed2006

Automated solid-phase extraction method for measuring urinary polycyclic aromatic hydrocarbon metabolites in human biomonitoring using isotope-dilution gas chromatography high-resolution mass spectrometry.

In order to perform comprehensive epidemiological studies where multiple metabolites of several PAHs are measured and compared in low-dose urine samples, fast and robust methods are needed to measure many analytes in the same sample. We have modified a previous method used for measuring polycyclic aromatic hydrocarbon (PAH) metabolites by automating the solid-phase extraction (SPE) and including an additional eight metabolites. We also added seven new carbon-13 labeled standards, which improves the use of isotope-dilution calibration. Our method included enzyme hydrolysis, automated SPE and derivatization with a silylating reagent followed by gas chromatography (GC), coupled with high-resolution mass spectrometry (HRMS). Using this method, we measured 23 metabolites, representing 9 parent PAHs, with detection limits in the low pg/mL range. All steps in the clean-up procedure were optimized individually, resulting in a method that gives good recoveries (69-93%), reproducibility (coefficient of variation for two quality control pools ranged between 4.6 and 17.1%, N>156), and the necessary specificity. We used the method to analyze nearly 3000 urine samples in the fifth National Health and Nutrition Examination Survey (NHANES 2001-2002).

Automation↗
PubMedDate not supplied

Automated solid-phase extraction and quantitative analysis of 14 phthalate metabolites in human serum using isotope dilution-high-performance liquid chromatography-tandem mass spectrometry.

Phthalates are industrial chemicals with many commercial applications. Because of their common usage, the general population is exposed to phthalates. A sensitive and selective analytical method is necessary to accurately determine the phthalate levels in serum. We improved our previously developed analytical method to measure nine phthalate metabolites in human serum by automating the solid-phase extraction (SPE) procedure and by including five additional phthalate metabolites: phthalic acid; mono-isobutyl phthalate, a metabolite of di-isobutyl phthalate; mono-(3-carboxypropyl) phthalate, a major oxidative metabolite of di-n-octyl phthalate; and mono-(2-ethyl-5-oxohexyl) phthalate and mono-(2-ethyl-5-hydroxyhexyl) phthalate, two oxidative metabolites of di-(2-ethylhexyl) phthalate. Automation of the SPE eliminated the human variation associated with the manual SPE, thus improving the reproducibility of the measurements. Additional wash steps during SPE produced cleaner extracts and resulted in higher recoveries (80-99%) than the manual SPE method. Furthermore, the automated SPE method allowed for the unattended extraction of samples, with a concomitant increase in sample throughput compared to the manual SPE method. The method is accurate, precise, and sensitive, with limits of detection in the low nanogram-per-milliliter range.

Carbon Isotopes↗
PubMed2006

Ion-pair solid-phase extraction and gas chromatography-mass spectrometric determination of acidic hydrolysis products of chemical warfare agents from aqueous samples.

The chemical warfare agents (CWA) degrade rapidly in aqueous samples and convert to acidic degradation products. Extraction and identification of the degradation products from complex matrices using simple sample preparation and sensitive detection and identification is the most important step in the off-site analysis of samples. In this present study, we report a simple sample preparation step based on ion-pair (IP) solid-phase extraction (SPE) for the extraction of acidic degradation products of CWA namely methyl, ethyl, propyl phosphonic acids, thiodiglycolic acid and benzilic acid. The analysis was performed on GC-MS in electron impact ionization mode. Three IP reagents triethylamine (TEA), tetrabutylammonium bromide (TBAB) and cetyltrimethyl ammonium bromide (CTAB) were used. The recoveries were estimated using the internal and external standard methods. The recovery of the compounds was almost negligible when TEA was used as IP reagent. The recoveries obtained when TBAB and CTAB were used as IP reagents were high and reproducible. The recovery of test chemicals is above 90%, except for methyl phosphonic acid and ethylphosphonic acid (20.6 +/- 3.2% and 35.8 +/- 2.5%, respectively). The minimum detection limits of the method were calculated for all chemicals in both full scan and selected ion monitoring modes. The test chemicals could be detected in microgram per litre quantities by the IP-SPE method.

Cetrimonium↗
PubMed2005

Serum protein profiling by miniaturized solid-phase extraction and matrix-assisted laser desorption/ionization mass spectrometry.

Serum profiling by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) holds promise as a clinical tool for early diagnosis of cancer and other human diseases. Sample preparation is key to achieving reproducible and well-resolved signals in MALDI-MS; a prerequisite for translation of MALDI-MS based diagnostic methods to clinical applications. We have investigated a number of MALDI matrices and several miniaturized solid-phase extraction (SPE) methods for serum protein concentration and desalting with the aim of generating reproducible, high-quality protein profiles by MALDI-MS. We developed a simple protocol for serum profiling that combines a matrix mixture of 2,5-dihydroxybenzoic acid and alpha-cyano-4-hydroxycinnamic acid with miniaturized SPE and MALDI-MS. Functionalized membrane discs with hydrophobic, ion-exchange or chelating properties allowed reproducible MALDI mass spectra (m/z 1000-12,000) to be obtained from serum. In a proof-of-principle application, SPE with chelating material and MALDI-MS identified protein peaks in serum that had been previously reported for distinguishing a person diagnosed with breast cancer from a control. These preliminary results indicate that this simple SPE/MALDI-MS method for serum profiling provides a versatile and scalable platform for clinical proteomics.

Blood Proteins↗
PubMed2001

Determination of Cremophor EL in plasma after sample preparation with solid phase extraction and plasma protein precipitation.

The non-ionic emulsifier Cremophor EL can be quantified using a special potentiometric titration technique with barium chloride activation and precipitation with sodium tetraphenylborate. The end point of the titration is indicated by an ionsensitive coated wire electrode which responds to an excess of tetraphenylborate ions. Sample preparation is necessary to quantify the excipient in plasma of patients receiving ciclosporin formulations with Cremophor EL (Sandimmun), since plasma proteins cause disturbances of the titration. Solid phase extraction was tested with various sorbent materials. Although some of the sorbents yielded good extraction rates of Cremophor EL from aqueous solutions, the extraction rates from plasma were significantly lower. Therefore, plasma protein precipitation with acetonitrile has been examined as an alternative to SPE and has been proved the superior method. Using the precipitation technique, a recovery rate of above 90% was achieved. Furthermore, the limit of detection from plasma was found to be 30 microg, in analogy to the determination from aqueous solutions. The combination of the plasma protein precipitation with the potentiometric titration allows quantitation and thus pharmakokinetic investigations of Cremophor EL in patients treated with Sandimmun after kidney-transplantation.

Animals↗
PubMed2006

Quantitative determination of 1,4-dioxane and tetrahydrofuran in groundwater by solid phase extraction GC/MS/MS.

Groundwater contamination by cyclic ethers, 1,4-dioxane (dioxane), a probable human carcinogen, and tetrahydrofuran (THF), a co-contaminant at many chlorinated solvent release sites, are a growing concern. Cyclic ethers are readily transported in groundwater, yet little is known about their fate in environmental systems. High water solubility coupled with low Henry's law constants and octanol-water partition coefficients make their removal from groundwater problematic for both remedial and analytical purposes. A solid-phase extraction (SPE) method based on activated carbon disks was developed for the quantitative determination of dioxane and THF. The method requires 80 mL samples and a total of 1.2 mL of solvent (acetone). The number of steps is minimized due to the "in-vial" elution of the disks. Average recoveries for dioxane and THF were 98% and 95%, respectively, with precision, as indicated by the relative standard deviation of <2% to 6%. The method quantitation limits are 0.31 microg/L for dioxane and 3.1 microg/L for THF. The method was demonstrated by analyzing groundwater samples for dioxane and THF collected during a single sampling campaign at a TCA-impacted site. Dioxane concentrations and areal extent of dioxane in groundwater were greater than those of either TCA or THF.

Chemistry Techniques, Analytical↗