Search PubMed⌕ Search

SEARCH · Search PubMed

Results for “Solid Phase Extraction”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 577 records · Page 32Linked to original sources

Simultaneous optimization of the solid-phase extraction of organochlorine and organophosphorus pesticides using the desirability function.

In a multi-response situation [solid-phase extraction (SPE) of 18 organochlorine and nine organophosphorus pesticides from aqueous solution], several response variables are considered, and the optimization problem is more complex than in the single response case. Experimental design combined with desirability function was applied for the optimization of the SPE of these pesticides in order to obtain optimum operating conditions for routine work. This multi-criterion approach was developed for the simultaneous optimization of multiple responses and it is simple, easy to apply and permits the user to make subjective judgments on the importance of each response. The desirability function is based on the search for a global optimum [D = f (Y1, Y2, ..., Yn)] by the transformation of the measured property to a dimensionless scale for each criterion. The experimental design strategy involved a central composite design. A compromise between conflicting goals, such as achievement of good yields with SPE recoveries of ca. 100% for a large number of analytes with inherent chemical differences, was found by means of the desirability function D.

Chromatography, Gas↗

Mixed-mode solid-phase extraction and cleanup procedures for the liquid chromatographic determination of thiabendazole and carbendazim in fruit juices.

Solid-phase extraction (SPE) procedures were developed for rapid cleanup and determination of thiabendazole and carbendazim in orange, apple, and grape juices. Samples were prepared by using an SPE cartridge containing a mixed-mode sorbent with both reversed-phase and strong cation-exchange chemistries. Analysis was by liquid chromatography with photodiode-array UV detection. Orange juice was analyzed by mixed-mode cation-exchange extraction with reversed-phase cleanup; the other juices were analyzed by reversed-phase extraction with cation-exchange cleanup. Recoveries >80% for carbendazim and >90% for thiabendazole. Quantitation limits were 20 microg/L for both analytes.

Benzimidazoles↗

Interlaboratory comparison of pesticide recovery from water using solid-phase extraction disks and gas chromatography.

An interlaboratory study was conducted to assess the suitability of C18 solid-phase extraction disks to retain and ship different pesticides from water samples. Surface and deionized water samples were fortified with various pesticides and extracted using C18 disks. Pesticides were eluted from disks and analyzed in-house, or disks were sent to another laboratory where they were eluted and analyzed. Along with the disks, a standard pesticide solution in methanol was also shipped to be used for fortification, extraction, and analysis. The highest recovery from deionized or surface water using shipped disks was obtained for cyanazine (>97%), followed by metalaxyl (>96%), and atrazine (>92%). Although <40% of the bifenthrin, chlorpyrifos, and chlorothalonil fortified in surface water was recovered from shipped disks, recoveries from deionized water were >70%. From in-house eluted disks, bifenthrin and chlorpyrifos were recovered at 118 and 105%, whereas chlorothalonil showed 71% recovery, indicating that poor recovery from surface water was due to loss during shipping rather than low retention by the C18 disks. There was no consistent relationship between recovery from C18 disk and physicochemical properties for the pesticides included in this study. For most of the 13 pesticides tested, there were no differences in recovery between in-house extracted disks and shipped disks, indicating the suitability of disks to concentrate and transport pesticides extracted from water samples.

Chemical Phenomena↗

Rapid analysis of momordicoside A in bitter melon by high performance liquid chromatography following solid phase extraction.

A rapid, simple and accurate method for the determination of momordicoside A has been established using solid phase extraction (SPE) followed by high performance liquid chromatography (HPLC). Sample was processed by SPE on a Carb cartridge (3 mL/250 mg), and was then determined by HPLC on a C18 column (4.6 mm i.d. x 250 mm, 5 microns) with V(acetonitrile):V(methanol):V(50 mmol/L potassium dihydrogen phosphate buffer) = 25:20:60 as mobile phase (0.8 mL/min) and UV detection at 208 nm. The calibration curves were linear from 10 mg/L to 1,000 mg/L (r2 = 0.9992). The analytical method was shown to be highly reproducible, giving all of the relative standard deviations and relative mean errors less than 10% for both intra-day and inter-day determinations. The absolute recoveries were greater than 90%.

Antineoplastic Agents, Phytogenic↗

[Solid-phase extraction and RP-HPLC screening procedure for diuretics, probenecid, caffeine and pemoline in urine].

A solid-phase extraction and reversed phase high performance liquid chromatographic method (RP-HPLC) was developed for the rapid determination of 13 diuretics (belonging to five different pharmacological groups), probenecid, caffeine and pemoline in urine. Two ml urine sample was first adsorbed on a XAD-2 column, then eluted with ether-ethyl acetate (1:1). The eluate was evaporated to dryness and reconstituted in methanol. The methanolic solution was injected into a HP LiChrosorb RP-18 column, using phosphate buffer (pH 3) and acetonitrile as the mobile phase and monitored at 216 nm, 230 nm, and 275 nm on a diode array ultraviolet detector. The extraction recoveries of 16 drugs were above 75%. The limits of detection ranged from 0.3-3.0 micrograms/ml of urine. All drugs were separately administered to healthy volunteers, positive urine samples were collected, and urinary excretion-time curves of some drugs were reported.

Adult↗

Pesticide monitoring of drinking water with the help of solid-phase extraction and high-performance liquid chromatography.

This paper describes the results of a comparison of extraction efficiency between a new polymeric sorbent for solid-phase extraction (SPE) and classical RP-18. Pesticides and their hydrophilic metabolites in the low ppb range have been chosen as target compounds to be extracted from large volume samples. The pesticides were separated using HPLC and detected by diode array detection. Furthermore, a method is presented regarding the determination of carbendazim in water, using SPE on a mixed RP/polymer phase and high-performance liquid chromatography. Recovery, working range, precision and the detection limit are presented.

Benzimidazoles↗

Determination of chlormequat and mepiquat in pear, tomato, and wheat flour using on-line solid-phase extraction (Prospekt) coupled with liquid chromatography-electrospray ionization tandem mass spectrometry.

A sensitive and selective method is presented for the simultaneous analysis of the pesticides chlormequat and mepiquat at trace levels in tomato, pear, and wheat flour. The method entails direct injection of the food extract onto an on-line solid-phase extraction (SPE) instrument (Prospekt) using a strong cation-exchange resin. Analyte separation and detection is done by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS). Surrogate standards (d9-chlormequat, d6-mepiquat) are employed to compensate for recovery losses and potential MS-MS signal suppression. The method achieves a limit of quantification for both cationic analytes at or below 5 microg/kg, and good intra- and inter-assay precision with mean variability values <7% over a concentration range up to 195 microg/kg. This study also addresses potential analyte carry-over in an SPE on-line system, as well as the robustness of the procedure and its applicability in routine quality control operations.

Calibration↗

Simultaneous determination of phenolic xenoestrogens by solid-phase extraction and high-performance liquid chromatography with fluorescence detection.

A highly sensitive and selective method for simultaneous determination of some hydroxyl group-containing endocrine disruptors, including bisphenol A (BPA), bisphenol B (BPB), bisphenol E (BPE), bisphenol F (BPF) and 4-nonylphenol (4-NP), was developed. The method consists of precolumn derivatization of the analytes, solid-phase extraction (SPE) and subsequent chromatographic analysis by high-performance liquid chromatography (HPLC) with fluorescence detection. 4,4'-Cyclohexylidenebisphenol (BPZ) was used as an internal standard. Derivatization was carried out using 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl) as a label. Parameters of the derivatization reaction (temperature, time, concentration of reagent, stability, etc.) and of the solid-phase extraction (recovery, solvent, etc.) were studied in detail. Detection limits of compounds studied in standard solutions ranged from 0.08-1.3 ppb (ng/ml). The proposed method was successfully applied to plastic samples; BPA was found in both polycarbonate and polyvinyl chloride plastics, while 4-NP was found in plastics made of polyvinyl chloride and another polymer.

Benzhydryl Compounds↗

Gas chromatographic determination of fatty acids contained in different lipid classes after their separation by solid-phase extraction.

A quick and successful procedure is presented for the separation of polar lipids, monoacylglycerols (MAGs), diacylglycerols and triacylglycerols (TAGs) and for fatty acid determination in the above-mentioned lipid fractions by gas chromatographic analysis, which was acceptable for physiological and nutrition studies. In the analysis of edible oils and biological tissue samples, lipid classes were separated and purified by solid-phase extraction (SPE) using an aminopropylsilica column. Fatty acids in the sn-2 position in edible oil TAGs were determined after previous 1,3-specific lipase hydrolysis and separation of 2-MAGs by SPE using an aminopropylsilica column. A preliminary study of the solid-phase extraction separation of lipid classes with stock standard solutions using styrene-divinylbenzene-methacrylate copolymer (Nexus), octadecylsilica (C18) and aminopropylsilica (NH2) was carried out and it was shown that NH2 was the best sorbent for the above-mentioned purpose.

Chromatography, Gas↗

Reversed-Phase Ion-Pair High-Performance Liquid Chromatographic Quantitation of Difethialone Residues in Whole-Body Rodents with Solid-Phase Extraction Cleanup.

A reversed-phase ion-pair high-performance liquid chromatographic method was developed for the determination of difethialone residues in laboratory rats (Rattus norvegicus). Difethialone was extracted from rat tissue with chloroform/acetone/formic acid. The extracts were cleaned up by a solid-phase extraction (SPE) procedure using both silica and aminopropyl SPE sorbents, concentrated, and analyzed by reversed-phase ion-pair high-performance liquid chromatography. Difethialone was quantitated via ultraviolet absorbance at 262 nm. A surrogate compound, brodifacoum, was used to correct for method performance. The mean surrogate-corrected recoveries for whole ground rodent fortified at 0.2, 1.0, and 20 µg/g difethialone were 92.3 +/- 7.7, 84.8 +/- 6.6, and 90.2 +/- 3.1%, respectively. The method limit of detection was 0.054 µg/g.

Journal Article↗

Sample preparation based on dynamic ion-exchange solid-phase extraction for GC/MS analysis of acidic herbicides in environmental waters.

The newly established enrichment technique, dynamic ion-exchange solid-phase extraction (DIE-SPE), was studied for sample preparation for GC/MS analysis of 16 acidic herbicides in environmental waters. C18 bonded silica was the solid-phase material used. The optimal sample pH was weakly acidic to neutral. However, for common tap water and surface water, which run pH 6-9, all the acidic herbicides except for Chloramben could be effectively extracted from a sample of 1,000-mL volume without pH adjustment. The humic acid could be concurrently extracted from water, but most of it was separated from the sample by using 3 mL of 10% methanol in acetone as the eluent, which would completely elute the analytes and leave a large part of the humic acid on the cartridge. The selective elution reduced the interference of humic acid and made the DIE-SPE an effective approach for the analysis of the acidic herbicides in surface water. Comparing DIE-SPE with conventional reversed-phase SPE (RP-SPE), the former gave higher recoveries for the acidic herbicides and was less affected by sample matrixes. A tandem-cartridge system combining RP- and DIE-SPE in sequence was set up for the simultaneous isolation of the acidic herbicides and removal of the interfering substances. Despite some minimal retention on the upper RP-SPE cartridge, most of the acidic herbicides could be extracted on the lower DIE-SPE cartridge with recovery over 80% except for Chloramben (50%), fenoprop (73%), MCPB (67%), and 2,4-DB (70%) when a 500-mL aqueous sample of pH 9.5 was percolated through the tandem-cartridge system. The effectiveness of the system in removing the long carbon chain fatty acids as well as the basic and neutral organic interfering substances from the sample was also demonstrated.

Acids↗

Validated high-performance liquid chromatographic method utilizing solid-phase extraction for the simultaneous determination of naringenin and hesperetin in human plasma.

Naringenin and hesperetin, the aglycones of the flavanone glucosides naringin and hesperidin occur naturally in citrus fruits. They exert a variety of pharmacological effects such as antioxidant, blood lipid-lowering, anticarcinogenic and inhibit selected cytochrome P-450 enzymes resulting in drug interactions. A specific, sensitive, precise, and accurate solid-phase extraction high-performance liquid chromatographic (HPLC) assay for the simultaneous determination of naringenin and hesperetin in human plasma was developed and validated. After addition of 7-ethoxycoumarin as internal standard, plasma samples were incubated with beta-glucuronidase/sulphatase, and the analytes were isolated from plasma by solid-phase extraction using C(18) cartridges and separated on a C(8) reversed phase column with methanol/water/acetic acid (40:58:2, v/v/v) as the eluent at 45 degrees C. The method was linear in the 10-300 ng/ml concentration range for both naringenin and hesperetin (r>0.999). Recovery for naringenin, hesperetin and internal standard was greater than 76.7%. Intra- and inter-day precision for naringenin ranged from 1.4 to 4.2% and from 1.9 to 5.2%, respectively, and for hesperetin ranged from 1.3 to 4.1% and from 1.7 to 5.1%, respectively. Accuracy was better than 91.5 and 91.3% for naringenin and hesperetin, respectively.

Chromatography, High Pressure Liquid↗

A simplified protein precipitation/mixed-mode cation-exchange solid-phase extraction, followed by high-speed liquid chromatography/mass spectrometry, for the determination of a basic drug in human plasma.

A simplified protein precipitation/mixed-mode cation-exchange solid-phase extraction (PPT/SPE) procedure has been investigated. A mixture of acetonitrile and methanol along with formic acid was used to precipitate plasma proteins prior to selectively extracting the basic drug. After vortexing and centrifugation, the supernatants were directly loaded onto an unconditioned Oasis MCX microElution 96-well extraction plate, where the protonated drug was retained on the negatively charged sorbent while interfering neutral lipids, steroids or other endogenous materials were washed away. Normal wash steps were deemed unnecessary and not used before sample elution. The sample extracts were analyzed under both conventional and high-speed liquid chromatography/tandem mass spectrometry (LC/MS/MS) conditions to examine the feasibility of the PPT/SPE procedure for human plasma sample clean-up. For the conventional LC/MS/MS method, chromatographic separation was achieved on a C18, 2.1 x 50 mm column with gradient elution (k' = 5.5). The mobile phase contained 0.1% formic acid in water and 0.1% formic acid in acetonitrile. For the high-speed LC/MS/MS method, chromatographic separation was achieved on a C18, 2.1 x 10 mm guard column with gradient elution (k' = 2.2, Rt = 0.26 min). The mobile phase contained 0.1% formic acid in water and 0.001% trifluoroacetic acid in acetonitrile. Detection for both conventional and high-speed LC/MS/MS methods was by positive ion electrospray tandem mass spectrometry on a ThermoElectron Finnigan TSQ Quantum Ultra, where enhanced resolution (RP 2000; 0.2 amu) was used for high-speed LC/MS/MS. The standard curve, ranging from 0.5 to 100 ng/mL, was fitted to a 1/x weighted quadratic regression model. This combined PPT/SPE procedure effectively eliminated time-consuming sorbent conditioning and wash steps, which are essential for a conventional mixed-mode SPE procedure, but retained the advantages of both PPT (removal of plasma proteins) and mixed-mode SPE (analyte selectivity). The validation results demonstrated that this PPT/SPE procedure was well suited for both conventional and high-speed LC/MS/MS analyses. In comparison with a conventional mixed-mode SPE procedure, the simplified PPT/SPE process provided comparable sample extract purity. This simple sample clean-up procedure can be applied to other basic compounds with minor modifications of PPT solvents.

Blood Proteins↗

Simultaneous extraction and analysis of 11 tetracycline and sulfonamide antibiotics in influent and effluent domestic wastewater by solid-phase extraction and liquid chromatography-electrospray ionization tandem mass spectrometry.

Wastewater treatment plants (WWTPs) in which antibiotic compounds are not totally eliminated are considered to be point sources of antibiotic contamination in surface and ground waters. Therefore, there is a need for sensitive and reliable analytical methods for measuring these compounds in WWTP water matrices. This paper describes a simultaneous method for the determination of six tetracyclines (TCs) (oxytetracycline (OTC), tetracycline (TC), demeclocycline (DMC), chlortetracycline (CTC), doxycycline (DXC), meclocycline (MCC)) and five sulfonamides (SAs) (sulfathiazole (STZ), sulfamethazine (SMT), sulfachloropyridazine (SCP), sulfamethoxazole (SMX) and sulfadimethoxine (SDM)) using solid-phase extraction followed by liquid chromatography-ion trap tandem mass spectrometry. The average recovery of 11 antibiotics for simultaneous extraction was 83.3+/-12.6 and 89.8+/-11.5% for six TCs, and 95.2+/-11.4 and 97.7+/-10.6% for five SAs in the influent and effluent water, respectively. Matrix effects were found to be significant when measuring TCs but not SAs. The accuracy and day-to-day variation of the method fell within an acceptable range of 15% absolute. Method detection limits in wastewater matrices were between 0.03 and 0.07 microg/L. For the investigated 11 antibiotic compounds TC, DMC, CTC, DXC, SMT, SMX and SDM were found in the influents with a concentration range of 0.05-1.09 microg/L. CTC, DXC and SMX were also detected in the effluents with a concentration range of 0.06-0.21 microg/L. These results were compared with those in WWTP effluents of Canada, Germany and Switzerland.

Anti-Bacterial Agents↗

Validation of a chromatographic method to determine E-6006 and its metabolite E-6332 in rat and dog plasma by solid-phase extraction and capillary gas chromatography. Application in pharmacokinetics.

E-6006, 5-(alpha-[2-(dimethylamino)ethoxy]-2-thienylmethyl)-1-methyl-1H-pyrazole is a new antidepressive compound and E-6332, 5-(alpha-[2-(methylamino)ethoxy]-2-thienylmethyl)-1-methyl-1H-pyrazole is its desmethylate metabolite. With the aim of quantifying E-6006 and E-6332, simultaneously in rat or dog plasma, a method of analysis based on solid-phase extraction coupled with capillary gas chromatographic system with N-P detection was developed and validated. E-6006, E-6332 and its internal standard (E-4018) were isolated from plasma using an off-line semiautomatic solid-phase extraction method. Gas chromatography separations were carried out by means of 12 m length, 0 2 mm (i.d.) and 0.33 microm (f.t.) ULTRA 1 type capillary column in splitless mode of injection at 190 degrees C, with a TSD or specific nitrogen--phosphorus detector. No peaks interfering with the quantification of E-6332 and E-6006 were observed. The limit of quantification was 5 ng/ml with a precision and accuracy <17%. The peak height ratios were proportional to E-6332 and E-6006 concentration over the range from 5 to 600 ng/ml (r(2)>0.998). Mean recoveries of E-6332, E-6006 and internal standard from rat plasma were between 57.1 and 82.6. Intra-assay precision coefficients were <8.0 and <11.8%, respectively, for E-6332 and E-6006, with an accuracy <12.6 and <9.7%. Both inter-assay precision and accuracy were within acceptable limits (<15%). In dog, the results were very similar to those obtained in rat. To show an example of the suitability of the method to determine E-6332 and E-6006, plasma profiles obtained after single oral and intravenous administration of 20 mg/kg to rats and 25 mg/kg to dogs are reported.

Animals↗

Determination of avilamycin A and B in pig faeces by solid phase extraction and reverse-phase HPLC assay.

A HPLC method is described for the simultaneous determination of avilamycin A and B in pig faeces, following extraction using acetonitrile and normal-phase solid phase extraction. The HPLC stationary phase was Kromosil 5 micro C-18 with a mobile phase of 48% acetonitrile and 52% 0.01N ammonium acetate buffer, pumped at a flow rate of 1 ml/min. Detection was by UV absorbance at 295 nm and an injection volume of 50 microl was used. Recovery from faeces was >98% and intra-assay precision (CV) was <9.0% for both compounds. The lowest limit of quantification was 0.9 mg/kg (avilamycin A) and 0.2 mg/kg (avilamycin B) with an accuracy of <15% error. No interference was seen from endogenous materials in pig faeces and commonly used veterinary antibiotics.

Animals↗

Quantitative determination of pharmaceuticals using nano-electrospray ionization mass spectrometry after reversed phase mini-solid phase extraction.

The pre-concentration effect of solid phase microextraction (SPE) with nano-electrospray ionization mass spectrometry (nano-ESI MS) for selected pharmaceuticals is presented. An analytical method is developed for the quantitative determination of dicyclomine in serum with cyclopentolate as the internal standard by off-line nano-ESI ion-trap MS with reversed phase mini-SPE. Homemade C18 and C4 mini-SPE cartridges of 0.5 and 1cm in length and 1.55 mm i.d. have been tested for pre-concentration of samples originally 30 microL in volume. After SPE, the volume of the sample in methanol is about 1-2 microL and 0.5 microL can be injected into the nano-ESI MS instrument. Use of a 1cm C18 cartridge lowered the detection limit of dicyclomine 100 times to 16.1 fmole. Dicyclomine spiked in serum can be determined by nano-ESI MS after protein precipitation and further clean-up on the 1cm C18 cartridge. However, the slope of a calibration curve of dicyclomine standards spiked in serum is more than a factor of 10 less than that for a calibration curve of dicyclomine standards prepared in water indicating pre-concentration of pharmaceuticals could be compromised by a complex biological matrix.

Animals↗