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PubMed2000

Low-carbon silica sorbents for solid-phase extraction.

The applicability of silica gels, modified with cyclic organosiloxanes, in solid-phase extraction (SPE) has been tested. Surface characteristics of the adsorbents prepared are determined by: elemental analysis, 29Si cross-polarisation magic angle spinning nuclear magnetic resonance spectroscopy (29Si CP MAS NMR) and diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy. The sorbents with low carbon contents are used for extraction of chlorinated pesticides, polychlorinated biphenyls and nitro-compounds from water. The properties of the sorbents are compared with commercial C18 ones. It is shown that the low-carbon silica SPE sorbents can ensure satisfactory recoveries and reveal some selectivity.

Adsorption↗
PubMed1994

Simultaneous measurement of the major metabolites of dolasetron mesilate in human urine using solid-phase extraction and high-performance liquid chromatography.

A method based on solid-phase extraction and high-performance liquid chromatography (HPLC) has been developed for the simultaneous quantitation of the principal active metabolites of dolasetron mesilate [i.e. MDL 74,156 (II), MDL 102,382 (III) and MDL 73,492 (IV)] in human urine. The method has been validated over the concentration range of 200-5000 pmol/ml for all three metabolites. Within-day and day-to-day coefficients of variation were less than 9 and 14%, respectively, for the three metabolites. The method allowed the simultaneous quantitation of III, IV and II and the evaluation of the urinary excretion of these metabolites in human urine following the administration of dolasetron mesilate.

Antiemetics↗
PubMed2001

Development of a generic method to the solid-phase extraction of acidic compounds from complex matrices.

A mixed-mode solid-phase extraction procedure was developed for the isolation and purification of acidic compounds from complex biological matrices. Urine samples were spiked with several acidic drugs and diluted in ammonium acetate buffer. Isolute HAX columns (a mixed-mode phase consisting of both hydrophobic and ion-exchange ligands) were conditioned with methanol and ammonium acetate prior to sample loading. Once the samples were loaded, the cartridges were rinsed sequentially with ammonium acetate and a 50:50 ratio of methanol and deionized water. The analytes were eluted with an 80:20 ratio of methanol and acetic acid. The eluates were evaporated to dryness and reconstituted to a final volume with a 98:2:0.1 ratio of deionized water, acetonitrile, and trifluoroacetic acid. Samples were analyzed by high-performance liquid chromatography. The absolute recoveries for most of the tested acidic drugs exceeded 80% at an original concentration of 1 microg/mL. Hydrophobic and ion-exchange sorbents were also investigated separately; however, the retention of the analytes suffered during sample application as well as the purity of the eluted extract. Results on anion-exchange columns show that the correct choice of counter-ion is extremely important to the retention of acidic analytes. The highest absolute recoveries were obtained when acetate was the counter-anion on the ion-exchange sorbent.

Carboxylic Acids↗
PubMed2003

HPLC determination of (+)-pseudoephedrine and (-)-ephedrine in Japanese herbal medicines containing Ephedra herb using solid-phase extraction.

We developed a rapid and simple HPLC method combined with solid-phase extraction (SPE) for quantitative analysis of (+)-pseudoephedrine (PEP) and (-)-ephedrine (EP) in Japanese herbal (Kampo) medicines such as Kakkon-to, Sho-seiryu-to, Goshaku-san and Bofu-tsusho-san. SPE was performed on TOYOPAK IC-SP M containing propylsulfonic groups. Determination of PEP and EP was carried out using ion-pair reversed-phase HPLC with sodium dodecyl sulfate. N-Benzyldiethylamine was used as an internal standard. The analytical procedure was validated with regard to specificity, linearity, accuracy, and precision. These data suggest that the analytical method developed in this study is useful for quantitative analysis of PEP and EP in various formulations of Kampo medicine containing Ephedra herb.

Chromatography, High Pressure Liquid↗
PubMed1996

[A new solid-phase extraction method for human urinary 3-methoxy-4-hydroxyphenylethyleneglycol].

A new solid-phase extraction procedure for urinary 3-methoxy-4-hydroxy-phenylethyleneglycol (MHPG) was established. Sep-Pak Diol cartridge was used, because MHPG is a neutral and alcoholic compound. Aqueous samples were adsorbed to the cartridge, then MHPG was eluted by the addition of ethyl acetate. After the eluate was evaporated, the residuum was dissolved with HPLC mobile phase and injected into HPLC. The extraction procedure was highly specific to MHPG, and none of other acidic catecholamine metabolites, such as vanillylmandelic acid (VMA), homovanillic acid (HVA) and 3,4-dihydroxyphenylacetic acid (DOPAC), was extracted. The recovery of MHPG using this method was over 90% and higher than those using previously described methods such as liquid-liquid extraction with ethyl acetate. Of the three vanillyl alcohol isomers, isovanillyl alcohol was the most suitable as an internal standard for the correction of column-to-column variation of the recovery. Human urinary unconjugated MHPG extracted by the new procedure could be measured by HPLC with a fluorescence detection. Further complicated derivatization and more sensitive detection systems, such as GC-MS and HPLC-electrochemical detector (ECD), were not needed due to high selectivity and high recovery of the extraction procedure. In addition, the urinary total (conjugated plus unconjugated) MHPG content could also be determined by the same procedure after an enzymatic hydrolysis of conjugated MHPG. The newly developed extraction procedure was simple, rapid and highly specific, and might be applicable to the analysis of MHPG in various body fluids.

Chromatography, High Pressure Liquid↗
PubMedDate not supplied

Determination of niacin in infant formula by solid-phase extraction and anion-exchange liquid chromatography.

A peer-verified, solid-phase extraction (SPE)/anion exchange liquid chromatographic method is presented for the determination of niacin in milk-based and soy-based infant formula. Analysis is in 3 steps: test sample digestion, extraction/cleanup, and liquid chromatography (LC). Digestion uses a standard AOAC digestion procedure that involves autoclaving at 121 degrees C for 45 min in (1 + 1) H2SO4 to free endogenous niacin from protein and to convert added niacinamide to niacin. The digest solution is adjusted to pH 6.5 with 7.5M NaOH. Acidification to pH <1.0 with (1 + 1) H2SO4 precipitates the protein. The clarified solution is then filtered, and the filtrate is brought to volume. SPE of niacin is accomplished by passing an aliquot of the digest solution through an aromatic sulfonic acid-SPE (ArSCX-SPE) column. After the column is washed with methanol and water to remove extraneous material, the niacin is eluted with 0.25M sodium acetate/acetic acid buffer at pH 5.6. An anion-exchange polystyrene-divinylbenzene column with 0.1 M sodium acetate/acetic acid buffer at pH 4.0 is used for LC. Niacin is determined by UV detection at 260 nm. A standard curve is prepared by passing known amounts of niacin through the ArSCX-SPE columns used for niacin extraction. The following values for x and relative standard deviation (RSD) were obtained for National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1846 Infant Formula with a certified value for niacin of 63.3 +/- 7.6 microg/g: Submitting laboratory.-- x = 59.7 +/- 4.0 microg/g; RSD = >6.7%; confidence interval (CI) = +/- 1.4 microg/g; n = 27. Peer laboratory.--x = 56.6 +/- 6.6 microg/g; RSD = >11.7%; CI =+/- 4.1 microg/g; n = 8.

Animals↗
PubMedDate not supplied

Syringe-cartridge solid-phase extraction method for patulin in apple juice.

A syringe-cartridge solid-phase extraction (SPE) method was developed for determination of patulin in apple juice. A 2.5 mL portion of test sample was passed through a conditioned macroporous SPE cartridge and washed with 2 mL 1% sodium bicarbonate followed by 2 mL 1% acetic acid. Patulin was eluted with 1 mL 10% ethyl acetate in ethyl ether and determined by reversed-phase liquid chromatography using a mobile phase consisting of 81% acetonitrile, 9% water, and 10% 0.05M potassium phosphate buffer, pH 2.4. Recoveries averaged 92% and the relative standard deviation was 8.0% in test samples spiked with 50 ng/mL patulin. The method appears to be applicable for monitoring apple juice samples to meet the U.S. Food and Drug Administration compliance action level of 50 microg/kg in an industrial quality assurance laboratory environment.

Beverages↗
PubMedDate not supplied

Florisil solid-phase extraction cartridges for cleanup of organochlorine pesticide residues in foods.

Florisil solid-phase extraction cartridges were evaluated for cleanup of organochlorine pesticide residues in food extracts. Elution patterns and recoveries were determined for 24 organochlorine pesticides. A range of elution solvents was evaluated. A 2% ethyl ether-petroleum ether eluant optimized overall recoveries while minimizing interferences from coextractants.

Animals↗
PubMed2006

Solid phase extraction, multidimensional gas chromatography mass spectrometry determination of four novel aroma powerful ethyl esters. Assessment of their occurrence and importance in wine and other alcoholic beverages.

A method for the quantitative determination of four powerful aromatic ethyl esters recently identified in some wines has been developed, validated and applied to the determination of these compounds in different samples of wine, whisky and brandy. Ethyl 2-, 3-, and 4-methylpentanoate and ethyl cyclohexanoate are extracted from 100ml of sample by solid phase extraction (SPE) on a 200mg LiChrolut EN bed. Major compounds are eliminated by rinsing with a water-methanol (50:50) solution containing 1% sodium bicarbonate, and analytes are eluted with 1.5ml of dichloromethane. Fifty microlitres of this extract are then injected in a multidimensional gas chromatography-mass spectromety (GC-GC-MS) system. Recoveries in the SPE are quantitative. Method repeatability is satisfactory (5-12% for a 5-10ngl(-1) level, and less than 7% for 25-50ngl(-1) level), the method linearity holds along the whole range of occurrence of analytes (2-2700ngl(-1)), and the signal is independent on the matrix. Method detection limits are below 1ngl(-1) in all cases. Results suggest that these compounds are formed by the slow esterification with ethanol of the corresponding acids formed by different microorganisms. The levels of these compounds are above the corresponding thresholds in most samples of aged wines or distillates, but are particularly high in some sweet wines, whiskeys and brandies where they may constitute the most important contributors to the sweet-fruity notes reaching concentrations up to 85-350 times higher than the corresponding odor thresholds.

Alcoholic Beverages↗
PubMed2005

Determination of eleutheroside E and eleutheroside B in rat plasma and tissue by high-performance liquid chromatography using solid-phase extraction and photodiode array detection.

A HPLC method with photodiode array detection (PDA) was developed for the determination and a pharmacokinetic study of eleutheroside E (ELU E) and eleutheroside B (ELU B) in rat plasma and tissue following an eleutherococcus injection. The analysis was performed on a Kromasil C18 column, using water-acetonitrile as the gradient mobile phase and 0.8 mL/min flow rate. Detection wavelengths of ELU E and ELU B were 220 and 206 nm, respectively. Protein from the biological sample was deposited using acetonitrile. ELU E and ELU B were extracted from the biological samples using acetonitrile, separated by solid-phase extraction, and eluted from the cartridge using 60% methanol. The extraction recovery of ELU E and ELU B was 91.2 and 88.8%, respectively. The limit of detection was 37.6 ng/mL for ELU E and 37.0 ng/mL for ELU B (S/N = 3) in plasma. Blood drug level-time cuvers of ELU E and ELU B in Wister rats following administration of an eleutherococcus injection into femoral vein were shown to fit a three-compartment model. The half-life (t1/2) was 4.662 h for ELU E and 2.494 h for ELU B. Following administration of a single eleutherococcus injection, the concentration of ELU E and ELU B in the tissue was Cliver > Ckidney > Cspleen > Cheart and Ckidney > Cliver > Cheart. We believe the method described in the present paper is accurate and reliable and can be used for pharmacokinetic studies of ELU E and ELU B in rats. In addition, the method for sample preparation, using solid phase extraction, is precise, simple and rapid.

Animals↗
PubMed1999

Improved validated assay for the determination of mefloquine and its carboxy metabolite in plasma, serum and whole blood using solid-phase extraction and high-performance liquid chromatography.

An improved high-performance liquid chromatography method using a low silanol activity octadecylsilica column and a solid-phase extraction technique is validated for the simultaneous analysis of mefloquine and its carboxy metabolite in whole blood, plasma and serum. An octadecylsilica column with high silanol activity is compared to a column of low activity in terms of pH dependent variability of chromatographic retention times for mefloquine and its carboxy metabolite. The low silanol activity column showed a relatively large mobile phase pH range where retention times for both components are consistent. The solid-phase extraction procedure consists of a simple protein precipitation step followed by sample concentration and extraction using a C18 membrane disk. The inter- and intra-assay variability for a therapeutic concentration of mefloquine (1000 ng/ml) is less than 2% in whole blood, plasma and serum while carboxymefloquine (1000 ng/ml) is 2.3% or less. At concentrations as low as 100 ng/ml the inter-assay variability is 6.2% or less for both analytes. This method shows a robust analytical procedure for the simultaneous analysis of mefloquine and its carboxy metabolite where precise measurements are useful in pharmacokinetic studies and in estimating drug compliance.

Antimalarials↗
PubMed1997

Simultaneous quantitation of sixteen organochlorine pesticides in drinking waters using automated solid-phase extraction, high-volume injection, high-resolution gas chromatography.

A method is described for the simultaneous determination of sixteen organochlorine pesticides in drinking water using automated solid-phase extraction followed by high-volume (80 microliters) capillary column gas chromatography using electron capture detection. The fully automated extraction method followed by high-volume injection permits rapid sample analysis compared to previously described procedures since no further pre-concentration of the analytes is necessary after they have been eluted from the octadecyl solid-phase extraction cartridge. The lowest detectable concentrations of the pesticides are between 1-5 ng l(-1), relative recoveries range from 92-105% in tap water spiked at 100 ng l(-1) and the relative standard deviations are in the range 5-12%.

Autoanalysis↗
PubMed1992

Solid-phase extraction with supercritical fluid elution as a sample preparation technique for the ultratrace analysis of flavone in blood plasma.

A new sample preparation technique, solid-phase extraction with supercritical fluid elution, was developed for the selective isolation of ultratrace levels of drugs from plasma. Plasma samples spiked with a drug were applied to octadecylsilane cartridges and the cartridges were then washed, briefly dried and directly fitted into cells for subsequent supercritical fluid elution. The absolute recovery was studied by using a radiolabeled model compound. The extraction selectivity was examined by chromatographing the extracts with a reversed-phase high-performance liquid chromatographic method with ultraviolet detection. The effects of extraction pressure and the length of capillary restrictors on drug recovery were examined in order to determine the optimal conditions for supercritical fluid elution. The performance of the method was compared to that of conventional solid-phase extraction in terms of recovery, selectivity, precision and accuracy of analysis. Flavone was used as the model compound and dog plasma as the biological matrix for these studies.

Animals↗
PubMed2002

[Determination of benzo[a]pyrene in mainstream smoke by solid-phase extraction and gas chromatography-mass spectrometry].

A novel method is suggested for the determination of benzo[a]pyrene in mainstream smoke. Extraction of Cambridge pads was cleaned up with methanol/n-heptane extraction system and silica solid-phase extraction (SPE). The eluted solution containing benzo[a]pyrene was evaporated gently to complete dryness with N2 flow, then reconstituted in 200 microL ethyl acetate for determination with gas chromatography-mass spectrometry selected ion monitoring (SIM). The proposed method had good results and precision for the separation of pyrene in complex matrices.

Benzo(a)pyrene↗
PubMed2003

Solid-state and multidimensional solution-state NMR of solid phase extracted and ultrafiltered riverine dissolved organic matter.

In this study we used multidimensional solution-state NMR to elucidate the differences in the chemical composition of solid phase extracted and ultrafiltered DOM isolates. DOM was isolated from water sampled from an oligotrophic river, the River Tagliamento (Italy). The recovery of total DOM was up to 42% with both isolation techniques. In addition to 1- and 2-D solution-state NMR, we also applied 1-D solid-state 13C NMR spectroscopy for DOM characterization. 13C NMR spectroscopy only produced broad overlapping resonances, thus allowing a bulk characterization of DOM composition. However, it demonstrated that the bulk chemical composition of the two DOM fractions exhibited minor spatial-temporal changes. The 2-D experiments (TOCSY, HMQC) showed that the solid phase extracted hydrophobic DOM contained predominantly aliphatic esters, ethers, and hydroxyl groups, whereas the ultrafiltered DOM was comprised partially of peptides/protein, with further evidence for a small amount of aliphatic/fatty acid material. Sugars were present in both DOM fractions. The results show the two isolation techniques selected for different suites of compounds within the bulk DOM pool.

Environmental Monitoring↗
PubMed2002

Extraction and separation of urinary catecholamines as their diphenyl boronate complexes using C18 solid-phase extraction sorbent and high-performance liquid chromatography.

The clinical utility of a one-step extraction procedure based on the retention of a diphenyl boronate-catecholamine complex on a C18 solid-phase extraction sorbent was investigated for the measurement of urinary catecholamines. Although recoveries with the extraction procedure were optimal over a relatively broad pH range (7.5-9.5), analytical factors such as sample loading and elution flow-rates, wash step and elution conditions, the concentration of catecholamines in urine to be extracted and the type of C18 sorbent used for extraction were found to influence the efficiency of this procedure and would therefore need to be controlled for optimal recoveries. Under optimal conditions the recovery of noradrenaline, adrenaline and dopamine from spiked urine was high and reproducible (mean recoveries were >85% for all catecholamines). The effectiveness of sample clean-up step was demonstrated by reverse phase, ion pair high-performance liquid chromatography with electrochemical detection. The method described was found to be suitable for the routine measurement of catecholamines in urine in clinical biochemistry laboratories. It has a high sample extraction throughput (40/h) and has adequate precision (between batch CV<8%) and sensitivity (LOD<30 nmol/l; LOQ<65 nmol/l) for all the catecholamines measured. The method has acceptable accuracy, showing a mean bias of 6.6% for noradrenaline, 7.3% for adrenaline and 6.8% for dopamine from the mean value of laboratories (N=69) participating in an External Quality Assurance scheme for greater than 12 months.

Boron Compounds↗
PubMed2000

Determination of nortriptyline in human serum by fully automated solid-phase extraction and on-line high-performance liquid chromatography in the presence of antipsychotic drugs.

A fully automated on-line method for determination of nortriptyline in human serum was developed using an ASPEC XL (Gilson) solid-phase extraction apparatus in combination with high-performance liquid chromatography. Solid phase extraction was performed on cyanopropyl cartridges. HPLC was carried out using a C18 column with a mobile phase of acetonitrile-0.01 M triethylamine (34:66 v/v) buffer, pH 3.0. UV detection was at 242 nm. The Inter-day CV% was <5%. Comparison with liquid-liquid extraction of serum from patients treated with nortriptyline showed good agreement. Studies of analytical interference from coadministered psychoactive drugs revealed that only imipramine and a methotrimeprazine metabolite interfered.

Antidepressive Agents, Tricyclic↗
PubMed1995

Development and validation of a high-sensitivity assay for an antipsychotic agent, CP-88,059, with solid-phase extraction and narrow-bore high-performance liquid chromatography.

An analytical method has been developed and validated for the quantitation of CP-88,059 in human serum. The compound and internal standard were extracted from serum by solid-phase extraction with a weak cation-exchange phase. The analytes were resolved from endogenous interferences using narrow-bore (2.1 mm I.D.) C18 reversed-phase HPLC. Column effluent was monitored by UV absorbance detection at 215 nm. The standard curve range was 1 to 250 ng/ml. The accuracy and precision values for the method were within +/- 10% and +/- 15%, respectively. A four-fold detectability enhancement was achieved using a 2.1 mm I.D. HPLC column relative to the more common 4.6 mm I.D. column. A performance comparison was made between the 2.1 mm I.D. column used for validation and a 4.6 mm I.D. column with the same stationary phase.

Antipsychotic Agents↗