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PubMed2001

Miniaturized solid-phase extraction with resin disks.

The properties and advantages of membrane disks for solid-phase extraction (SPE) are described. Miniaturization is a trend in SPE, as well as chemical analysis in general. A semimicro method is reviewed in which an extraction disk 4 mm in diameter is used for SPE. Even smaller scale separations are possible with a device in which a membrane 0.7 mm in diameter was incorporated into the needle of a 50-micro syringe. Aqueous samples containing 10 ppb of eight substituted benzenes were passed through the miniaturized-SPE syringe automatically using a single-syringe infusion pump. Elution volumes of 5 microl provided 500-fold concentrations and delivered average recoveries greater than 90% and an average relative standard deviation (RSD) of 4.6% for the analytes. Direct injection of the 5 microl eluate from the miniaturized-SPE syringe into a gas chromatograph also produced average recoveries greater than 90% and an average RSD of 6.2%.

Benzene Derivatives↗
PubMed1997

Optimizing recoveries of two chlorotriazine herbicide metabolites and 11 pesticides from aqueous samples using solid-phase extraction and gas chromatography-mass spectrometry.

A method was developed for solid-phase extraction of two chlorotriazine herbicide metabolites, deethylatrazine (DEA) and deisopropylatrazine (DIA), from aqueous samples. Two C18 phases in cartridge format were compared and recoveries were found to be highly sensitive to sorbent amount, sample volume and presence of parent compounds. Recoveries were significantly improved using a partially non-endcapped C18 phase compared to the normal C18 phase, particularly for DIA, apparently due to polar interactions. Combinations of sample volume and sorbent amount were tested using deionized water to determine an optimal combination of 200 ml and 1.0 g, respectively. Recoveries from a variety of river, stream, runoff and ground waters averaged 105-116% and 109-117% at concentrations of 0.5-1.0 ng/ml for DIA and DEA, respectively, with minimum detection limits of 0.05 ng/ml. Other pesticides tested also have acceptable recoveries using this method.

Atrazine↗
PubMed2006

Semiautomated determination of pesticides in water using solid phase extraction disks and gas chromatography-mass spectrometry.

A method based on semiautomated solid phase extraction using octadecyl-bonded silica disks and gas chromatography-mass spectrometry, operated in selected ion monitoring mode, allows detection and quantification of approximately 100 pesticides and transformation products in drinking water. Samples (500 mL) were passed through the disk, and the retained pesticides were eluted with acetone and ethyl acetate. Typical recoveries for pesticides at 0.1 microg L(-1) in water were in the range of 72-120% with relative standard deviations less than 20%. Calibration curves were linear over the range of 0.025-0.5 microg mL(-1) (equivalent to a concentration range in drinking water of 0.05-1.0 microg L(-1)).

Autoanalysis↗
PubMedDate not supplied

Determination of naltrexone and 6-beta-naltrexol in plasma by solid-phase extraction and gas chromatography-negative ion chemical ionization-mass spectrometry.

Solid-phase extraction (SPE) and a one-step derivatization are combined with gas chromatography-negative ion chemical ionization-mass spectrometry to simplify a previously reported method for the determination of naltrexone and its metabolite, 6-beta-naltrexol, in human plasma. Deuterated isotopomers of naltrexone and 6-beta-naltrexol are used as internal standards. After SPE, the extracts are derivatized with pentafluoropropionic anhydride at room temperature to form predominantly the bispentafluoropropionyl derivative of naltrexone and the trispentafluoropropionyl derivative of 6-beta-naltrexol. The derivatized extracts are analyzed by monitoring ion currents at m/z 633 (naltrexone), m/z 636 (naltrexone-2H3), m/z 633 6-beta-naltrexol), and m/z 640 (6-beta-naltrexol-2H7). Control plasma samples containing 0.3, 3, or 30 ng/nl of each analyte were analyzed for precision and accuracy with the following results: intra-assay, the percentage of target concentrations were 107-113% for naltrexone and 107-120% for 6-beta-naltrexol, and the coefficients of variation (CVs) were 3.1-6.3% for naltrexone and 3.1-5.7% for 6-beta-naltrexol; interassay, the percentage of target concentrations were 103-110% for naltrexone and 110-113% for 6-beta-naltrexol, and the CVs were 6.1-9.1% for naltrexone and 5.9-9.1% for 6-beta-naltrexol. At the limit of quantitation (LOQ) of 0.1 ng/ml, both analytes quantified within 20% of the target concentration with CVs less than 17%. The extraction recoveries determined at 0.3 and 30 ng/ml were 79 and 80% for naltrexone and 76 and 75% for 6-beta-naltrexol. Bench-top stability tested with concentrations of 0.3 and 3.0 ng/ml did not decrease more than 10% from the zero-hour controls at 3, 6 and 24 h. Selectively was determined using plasma from six donors and none showed interfering peaks greater than 22% of the LOQ for naltrexone and 53% of the LOQ for 6-beta-naltrexol. Using this method, naltrexone and 6-beta-naltrexol were readily detected in plasma specimens collected 5.5 h after oral doses of 25 or 100 mg naltrexone. Following discontinuation of treatment, naltrexone was detected 30 h after the 100-mg dose, whereas 6-beta-naltrexol was detected 125 h after both the 25- and 100-mg doses.

Drug Stability↗
PubMed1998

Improved solid-phase extraction of methadone and its two major metabolites from whole blood.

A solid-phase extraction (SPE) method for the efficient extraction of methadone and its two major metabolites, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine and 2-ethyl-5-methyl-3,3-diphenyl-1-pyrroline, from whole blood is described. The procedure combines extraction on Isolute Confirm HCX mixed-mode SPE columns and gas chromatographic-mass spectrometric analysis with deuterated methadone as the internal standard. The optimum extraction conditions for all three analytes were determined using spiked whole blood. The developed method is easier and faster than current liquid-liquid extraction (LLE) procedures and produces cleaner extracts. Calibration curves were linear from 0 to 600 ng/mL (r2 > 0.99) with recoveries greater than 90% for all three analytes. The concentrations of methadone and its metabolites in postmortem blood were determined in fatal cases using the developed SPE method and were found to compare well with results obtained using LLE.

Chemistry Techniques, Analytical↗
PubMedDate not supplied

Determination of methylparaben in o/w emulsions by solid-phase extraction and high-performance liquid chromatography.

A simple, fast, and accurate solid-phase extraction (SPE) using a 1-cc Oasis HLB cartridge for sample clean-up followed by an HPLC analysis for the assay of methylparaben (MP) in an o/w emulsion is described. One milliliter of methanol followed by 1 ml of 10% methanol in water was used to activate the cartridge sorbent. The sample was loaded into the cartridge and MP was then separated from oil-soluble excipients by washing the cartridge with 1 ml of 10% CH(3)CN in water. MP was finally eluted from the cartridge with mobile phase, acetonitrile and water (60:40), and quantified by HPLC analysis on a Nova-pak(R) C-18 column at 254 nm.

Chromatography, High Pressure Liquid↗
PubMed1997

Quantification of ketoprofen enantiomers in human plasma based on solid-phase extraction and enantioselective column chromatography.

An HPLC method for the quantification of ketoprofen enantiomers in human plasma is described. Following extraction with a disposable C18 solid-phase extraction column, separation of ketoprofen enantiomers and I.S. (3,4-dimethoxy benzoic acid) was achieved using a chiral column [Chirex 3005; (R)-1-naphthylglycine 3,5-dinitrobenzoic acid] with the mobile phase, 0.02 M ammonium acetate in methanol, set at a flow-rate of 1.2 ml/min. Baseline separation of ketoprofen enantiomers and I.S., free from interferences, was achieved in less than 20 min. The calibration curves (n = 14) were linear over the concentration range of 0.16 to 5.00 micrograms/ml per enantiomer [mean r2 of 0.999 for both enantiomers, root mean square error were 0.015 for R(-) and 0.013 for S(+)]. The inter-day coefficient of variation for duplicate analysis of spiked samples was less than 7% and the accuracy was more than 93% over the over the concentration range of 0.2 to 4.0 micrograms/ml for individual enantiomer using 1 ml of plasma sample. This method has been applied to a pharmacokinetic study from healthy human volunteers following the administration of a ketoprofen extended release product (200 mg). This method is simple, fast and should find wide application in monitoring pharmacokinetic studies of ketoprofen.

Anti-Inflammatory Agents, Non-Steroidal↗
PubMed2005

[Study on solid phase extraction spectrophotometric determination of zinc with 2-(2-quinolylazo)-5-dimthylaminophenol].

A highly sensitive, selective and rapid method for the determination of zinc based on the rapid reaction of zinc(II) with 2-(2-quinolylazo)-5-dimthylaminophenol (QADMAP) and the solid phase extraction of zinc ion with anion exchange resin cartridge was developed. In the presence of pH 8.5 buffer solution and Triton X-100 medium, QADMAP can react with zinc(II) to form a stable 2 :1 complex (QADMAP:Zn(II)). The molar absorptivity is 1.22 x 10(5)L x moL(-1) x cm(-1) at 590 nm. Beer's law is obeyed in the range of 0-1.0 microg x mL(-1). The zinc ions in the samples can be enriched and separated by solid phase extraction with anion exchange resincartridge. Testing results show that recovery for zinc(II) was from 95% to 104%, and RSD was below 3%. This method was applied to the determination of zinc in water and food with good results.

Aza Compounds↗
PubMed2000

Determination of methotrexate in human urine at trace levels by solid phase extraction and high-performance liquid chromatography/tandem mass spectrometry.

For biological monitoring of hospital personnel occupationally exposed to antineoplastic agents, highly sensitive and specific methods are required. In order to detect trace MTX urinary concentrations, a precise and accurate high-performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) procedure, incorporating solid phase extraction, has been developed. Urine samples were purified by solid phase extraction (SPE) on octadecyl bonded, endcapped silica SPE columns. After eluting with methanol, the solvent was evaporated obtaining a 25-fold concentration of the analyte. This procedure was validated by using 7-OHMTX as internal standard. Calibration curves had correlation coefficients always higher than 0.999, and the limit of detection was assessed at 0.2 microg L(-1). High specificity of the HPLC-MS/MS technique assures that no interfering substances are detected rather than the analyte of interest.

Antimetabolites, Antineoplastic↗
PubMed2001

Automated solid-phase extraction method for the determination of atovaquone in capillary blood applied onto sampling paper by rapid high-performance liquid chromatography.

A bioanalytical method for the determination of atovaquone in 100 microl blood-spots by solid-phase extraction and high-performance liquid chromatography has been developed and validated. Atovaquone was extracted from the sampling paper in 0.2 M phosphoric acid and a structurally similar internal standard was added with acetonitrile before being loaded onto a C8 end-capped solid-phase extraction column. Atovaquone and internal standard were analysed by high-performance liquid chromatography on a C18 J'Sphere ODS-M80 (150 x 4.0 mm) column with mobile phase acetonitrile-phosphate buffer, 0.01 M, pH 7.0 (65:35, v/v) and UV detection at 277 nm. The intra-assay precision was 2.7% at 12.00 microM and 13.5% at 1.00 microM. The inter-assay precision was 3.3% at 12.00 microM and 15.6% at 1.00 microM. The lower limit of quantification was 1.00 microM. The limit of detection was 0.50 microM.

Antifungal Agents↗
PubMed1998

Improved one-step solid-phase extraction method for morphine, morphine-3-glucuronide, and morphine-6-glucuronide from plasma and quantitation using high-performance liquid chromatography with electrochemical detection.

This communication describes an improved one-step solid-phase extraction method for the recovery of morphine (M), morphine-3-glucuronide (M3G), and morphine-6-glucuronide (M6G) from human plasma with reduced coextraction of endogenous plasma constituents, compared to that of the authors' previously reported method. The magnitude of the peak caused by endogenous plasma components in the chromatogram that eluted immediately before the retention time of M3G has been reduced (approximately 80%) significantly (p < 0.01) while achieving high extraction efficiencies for the compounds of interest, viz morphine, M6G, and M3G (93.8 +/- 2.5, 91.7 +/- 1.7, and 93.1 +/- 2.2%, respectively). Furthermore, when the improved solid-phase extraction method was used, the extraction cartridge-derived late-eluting peak (retention time 90 to 100 minutes) reported in our previous method, was no longer present in the plasma extracts. Therefore the combined effect of reducing the recovery of the endogenous components of plasma that chromatographed just before the retention time of M3G and the removal of the late-eluting, extraction cartridge-derived peak has resulted in a decrease in the chromatographic run-time to 20 minutes, thereby increasing the sample throughput by up to 100%.

Analgesics, Opioid↗
PubMedDate not supplied

Solid-phase extraction in amphetamine and methamphetamine analysis of urine.

A systematic evaluation that compares the recoveries of methamphetamine and amphetamine from spiked urine using C8, C18, strong cation exchanger (SCX), and C8-SCX mixed procedures (solid-phase extraction) is reported. Optimized experimental conditions including pH of the sample, solvent composition, and urine concentration for different solid-phase extraction sorbents were studied. The largest recoveries--greater than 86% for methamphetamine and greater than 88% for amphetamine--were achieved with a mixed adsorbent (C8-SCX) and mixed elution solvent CH2Cl2-i-propanol-NH4OH (78:20:2) at pH 6. The concentration of the urine matrix did not affect the extraction efficiency. The detection limits of methamphetamine and amphetamine in urine were obtained at 0.03 and 0.07 micrograms/mL, respectively, using gas chromatographic-mass spectrometric analysis operated in the electron impact mode.

Adsorption↗
PubMedDate not supplied

Analysis of fenthion in postmortem samples by HPLC with diode-array detection and GC-MS using solid-phase extraction.

Fenthion (O,O-dimethyl-O-[3-methyl-4-(methylthio)-phenyl]-thiophos-phate ) is an organophosphate insecticide. A specific method to quantitate fenthion in postmortem matrices with solid-phase extraction combined with high-performance liquid chromatography-diode-array detection (HPLC-DAD) and gas chromatography-mass spectrometry (GC-MS) is presented. Fenitrothion (O,O-dimethyl-O-[3-methyl-4-nitrophenyl]-thiophosphate) is selected as the internal standard. For sample cleanup, a simple but selective solid-phase extraction is chosen after comparison with traditional liquid-liquid extraction procedures. Homogenized and appropriately diluted aqueous samples are applied, and the analytes are desorbed with 5 mL of dichloromethane. Aliquots of the extract are used for HPLC-DAD and GC-MS analysis, Liquid and GC conditions are as follows: gradient elution with a mixture of methanol and water (10:90 to 90:10, v/v) containing 0.0125M NaOH on an Aluspher RP-Select B column monitoring at 250 nm, and temperature programming from 60 to 300 degrees C on a dimethylpolysiloxane column in the SCAN mode, respectively. This method is applied to a suicidal case involving unsuspected acute intoxication with fenthion (concentration in blood, 3.8 micrograms/mL).

Aged↗
PubMed1998

On-line coupling of solid-phase extraction to gas chromatography with mass spectrometric detection to determine pesticides in water.

A group of pesticides with different chemical structures was determined in water by on-line coupling of solid-phase extraction to gas chromatography with mass spectrometric detection through an on-column interface. A 10 mm x 2 mm I.D. precolumn packed with PLRP-S was selected for the solid-phase extraction process. The parameters affecting the transfer of the analytes from the precolumn to the GC system (e.g. flow-rate, temperature and solvent vapor exit time) were optimized. An organic modifier was added to the sample before the extraction process to avoid adsorption problems. The use of the MS detector under selected ion monitoring acquisition enabled the analytes to be quantified at sub microgram-per-litre levels preconcentrating only 10 ml of sample, and the limits of detection (S/N = 3) were between 2 and 20 ng l-1. The method was applied to the determination of the pesticides in tap and river water, and molinate was determined in Ebro river water.

Gas Chromatography-Mass Spectrometry↗
PubMed2001

Solvent and solid-phase extraction of natural and synthetic anabolic steroids in human urine.

Liquid-liquid (using dichloromethane) and liquid-solid extraction processes (using disposable C18 cartridges) were applied to human urine samples spiked with 15 androgenic anabolic steroids (natural and synthetic). The extraction recoveries were assessed from different HPLC separations of anabolic steroids using water-acetonitrile mobile phase, and using calibration graphs obtained by injection into HPLC of standard samples of these compounds before and after extraction. The procedures, including sample preconcentration, showed extraction efficiencies over 90% which were independent on a wide range of concentrations tested. Solid phase extraction yielded poor results for oximetolone, danazol and dehydroepiandrosterone. For real urine samples, hydrolysis using beta-glucuronidase and washing using sodium hydroxide before and after solvent extraction, respectively, is recommended.

Acetonitriles↗
PubMed2006

High sensitivity assays for docetaxel and paclitaxel in plasma using solid-phase extraction and high-performance liquid chromatography with UV detection.

BACKGROUND: The taxanes paclitaxel and docetaxel have traditionally been used in high doses every third week in the treatment of cancer. Lately there has been a trend towards giving weekly low doses to improve the therapeutic index. This article describes the development of high performance liquid chromatographic (HPLC) methods suitable for monitoring taxane levels in patients, focusing on patients receiving low-dose therapy. METHODS: Paclitaxel and docetaxel were extracted from human plasma by solid phase extraction, and detected by absorbance at 227 nm after separation by reversed phase high performance liquid chromatography. The methods were validated and their performance were tested using samples from patients receiving paclitaxel or docetaxel. RESULTS: The limits of quantitation were 1 nM for docetaxel and 1.2 nM for paclitaxel. For both compounds linearity was confirmed from the limit of quantitation up to 1000 nM in plasma. The recoveries ranged between 92% and 118% for docetaxel and between 76% and 104% for paclitaxel. Accuracy and precision were within international acceptance criteria, that is within +/- 15%, except at the limit of quantitation where values within +/- 20% are acceptable. Low-dose patients included in an on going clinical trial had a median docetaxel concentration of 2.8 nM at 72 hours post infusion. Patients receiving 100 mg/m2 of paclitaxel had a mean paclitaxel concentration of 21 nM 48 hours after the end of infusion. CONCLUSION: We have developed an HPLC method using UV detection capable of quantifying 1 nM of docetaxel in plasma samples. The method should be useful for pharmacokinetic determinations at all relevant doses of docetaxel. Using a similar methodology paclitaxel can be quantified down to a concentration of 1.2 nM in plasma with acceptable accuracy and precision. We further demonstrate that the previously reported negative influence of Cremophor EL on assay performance may be overcome by degradation of the detergent by incubation with lipase.

Antineoplastic Agents↗
PubMed1997

Efficient high-performance liquid chromatographic assay for the simultaneous determination of metoprolol and two main metabolites in human urine by solid-phase extraction and fluorescence detection.

An improved, more efficient method for the determination of metoprolol and its two metabolites in human urine is reported. The simultaneous analysis of the zwitterionic metoprolol acidic metabolite (III, H117/04) with the basic metabolites alpha-hydroxymetoprolol (II, H119/66), metoprolol (I) and guanoxan (IV, internal standard) was achieved employing solid-phase extraction and isocratic reversed-phase HPLC. The analytes were extracted from urine (100 microliters) using C18 solid-phase extraction cartridges (100 mg), and eluted with aqueous acetic acid (0.1%, v/v)-methanol mixture (40:60, v/v, 1.2 ml). The eluents were concentrated (250 microliters) under vacuum, and aliquots (100 microliters) were analysed by HPLC with fluorescence detection at 229 nm (excitation) and 309 nm (emission) using simple isocratic reversed-phase HPLC (Novapak C18 radial compression cartridge, 4 microns, 100 x 5 mm I.D.). Acetonitrile-methanol-TEA/phosphate buffer pH 3.0 (9:1:90, v/v) was employed as the eluent (1.4 ml/min). All components were fully resolved within 18 min, and the calibration curves for the individual analytes were linear (r2 > or = 0.996) within the concentration range of 0.25-40.0 mg/ml. Recoveries for all four analytes were greater than 76% (n = 4). The assay method was validated with intra-day and inter-day variations less than 2.5%.

Administration, Oral↗
PubMed2004

Automated solid-phase extraction method for the determination of piperaquine in capillary blood applied onto sampling paper by liquid chromatography.

A bioanalytical method for the determination of piperaquine in 100 microL blood applied onto sampling paper, by solid-phase extraction and liquid chromatography, has been developed and validated. Blood spots were cut into small pieces prior to addition of 0.3M perchloric acid, acetonitrile and phosphate buffer containing an internal standard. The liquid phase was loaded onto a mixed phase cation-exchange (MPC) solid-phase extraction column. Piperaquine and the internal standard were analysed by liquid chromatography and separated on a Chromolith Performance (100 mm x 4.6 mm) column with acetonitrile:phosphate buffer pH 2.5, I = 0.1 (8:92, v/v) at the flow of 3.5 mL/min. The UV detection was performed at 345 nm. The intra-assay precision was 12.0% at 0.150 microM, 7.3% at 1.25 microM and 7.3% at 2.25 microM. The inter-assay precision was 1.8% at 0.150 microM, 5.2% at 1.25 microM and 2.8% at 2.25 microM. The lower limit of quantification (LLOQ) was determined to 0.050 microM where the precision was 14.7%.

Antimalarials↗