Solid-phase extraction as a tool to remove impurities and small fragments from synthetic peptides.
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Chemical Fractionation↗
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Determination of antibiotic substances in hospital sewage water using solid phase extraction and liquid chromatography/mass spectrometry and group analogue internal standards.
A method for determination of antibiotics in hospital sewage water has been developed and validated. Analogue internal standards for fluoroquinolones, sulfonamides, trimethoprim, beta-lactams (penicillins and cephalosporins), nitroimidazoles and tetracyclines were successfully used for calibration and shown to generally improve precision compared to external calibration. Matrix components caused ion suppression/enhancement effects during the MS detection for all analytes studied. Two effects were observed: general suppression and short-term variations in the MS response. In the hospital sewage water large temporal variations in the analyte concentration were observed during the course of the sampling period (seven grab samples in 13 h). Analyte concentrations varied within the following ranges (in microg l(-1)): ciprofloxacin, 3.6-101.0; metronidazole, 0.1-90.2; sulfamethoxazole, 0.4-12.8; ofloxacin, 0.2-7.6; trimethoprim, 0.6-7.6; and doxycycline, 0.6-6.7.
Anti-Bacterial Agents↗
Simultaneous determination of semivolatile organic compounds in indoor air by gas chromatography-mass spectrometry after solid-phase extraction.
A method is described for simultaneous determination of semivolatile organic compounds (SVOCs) in indoor air by gas chromatography-mass spectrometry (GC-MS). The selected 73 SVOCs were collected using combined adsorbents (quartz fiber filter disk and Empore disk) for 24 h at a 5.0 l/min flow rate. The SVOCs collected were extracted with acetone, concentrated, then analyzed by an internal standard method. Forty compounds (19 plasticizers and flame retardants; 19 insecticides; 1 synergist; and 1 fungicide) among the target SVOCs were determined accurately and precisely. The method of detection limits for these compounds were approximately 0.5 ng/m3 for most of the SVOCs. The collected SVOC samples could be stored for up to 1 month at 4 C in the refrigerator.
Calibration↗
Simultaneous determination of fluoroquinolone, sulfonamide, and trimethoprim antibiotics in wastewater using tandem solid phase extraction and liquid chromatography-electrospray mass spectrometry.
A robust and sensitive method for the detection of fluoroquinolones, sulfonamides and trimethoprim has been developed. Wastewater samples were acidified and extracted through an anion-exchange cartridge in tandem with a hydrophilic-lipophilic balance (HLB) cartridge, a procedure that reduced interferences from wastewater organic matter. The extracted antibiotics were analyzed using liquid chromatography electrospray mass spectrometry and selected ion monitoring. Quantification of antibiotics was assessed both by internal standard and standard addition methods. Average recoveries for a range of wastewater matrices were 37 to 129% for a 1 microg/L spiking concentration. The method detection limits (MDLs) of antibiotics in deionized water, final and secondary effluent ranged from 2 to 7 ng/L, from 20 to 50 ng/L, and from 30 to 90 ng/L, respectively. Assessment of matrix interference shows that signal suppression and MDL increases with higher amounts of organic matter in the sample. Analyses of samples from two municipal wastewater treatment plants indicate that ciprofloxacin, ofloxacin, sulfamethoxazole and trimethoprim are present in the secondary effluents at median concentrations of 100-160, 205-305, 395-575, and 40-705 ng/L, respectively.
Algorithms↗
Determination of free molecular phenolics and catechins in wine by solid phase extraction on polymeric cartridges and liquid chromatography with diode array detection.
The use of HLB Oasis polymeric cartridges to extract phenolic acids and aldehydes from red wines has been assayed and compared with the combination of ODS and SAX cartridges. The recoveries on the polymeric cartridges resulted to be notably higher with good precisions. The best operation conditions (cartridge conditioning, sample volume, clean-up and elution) for these latter were selected by experiments carried out on a synthetic wine sample spiked with 14 compounds and on red wine samples. A matrix-matched calibration was advisable to reduce the influence of the matrix in the quantification of the analytes as it was verified from the application of standard addition calibrations on several wine samples. Determination of the analytes in the extracts was performed by reversed-phase HPLC using mobile-phase and flow gradients and detection at 250, 280 and 340 nm.
Calibration↗
Solid-phase extraction gas chromatography-ion trap-mass spectrometry qualitative method for evaluation of phenolic compounds in virgin olive oil and structural confirmation of oleuropein and ligstroside aglycons and their oxidation products.
Phenolic compounds in Spanish virgin olive oil were analyzed by GC-MS after an SPE diol cartridge extraction and clean-up procedure. Posterior derivatization to trimethylsilyl (TMS) ethers using a mixture of hexamethyldisilazane:dimethylclorosilane (HMDS:DMCS) in pyridine (3:1:9) was performed. Several compounds were detected and 21 of them were identified. Free phenols such as hydroxytyrosol, tyrosol, tyrosyl and hydroxytyrosyl acetate, and aldehydic and dialdehydic forms of elenolic acid linked to tyrosol and hidroxytyrosol were the most abundant compounds. Likewise, oxidation products coming from the aldehydic and dialdehydic forms of elenolic acid, and of ligstroside and oleuropein aglycons, were detected, and their structure confirmed by other mass spectrometry technique, i.e., HPLC-APCI-MS. Individual oxidation products were isolated from an oxidized sample by preparative HPLC, converted to TMS ethers and re-analyzed by GC-MS. When necessary and for identification purposes, selective ion monitoring, namely, GC-MS-SIM, was employed. This is the first time that structures of oxidized forms are determined by GC-MS.
Gas Chromatography-Mass Spectrometry↗
Development of a multiresidue method for analyzing herbicide and fungicide residues in bovine milk based on solid-phase extraction and liquid chromatography-tandem mass spectrometry.
This report describes a liquid chromatography (LC)-tandem mass spectrometry (MS) multiresidue method for determining traces of 30 base/neutral/acid herbicides and fungicides in bovine whole milk. Four milliliters of milk was spiked with the analytes and two surrogate analytes (SAs) and then diluted with 35 mL of a water/methanol solution (50:50, v/v). This mixture was passed through a 0.5-g Carbograph 4 cartridge. After washings, analytes were re-extracted by back-flushing the cartridge with 1.5 mL of methanol followed by 6 mL of methylene chloride/methanol (80:20, v/v), 50 mmol/L formic acid. After partial solvent removal down to about 0.1, 0.15 mL of 1 mmol/L formic acid aqueous solution and an internal standard (IS) were added. After filtration, 50 microL of the final extract was then introduced into the LC analytical column. During the chromatographic run, the MS system was operated in both positive and negative ion modes. MS data acquisition was performed in the multi-reaction monitoring mode, selecting two precursor ion>product ion transitions for each target compound, except for pentachlorophenol. On analyzing six milk samples from different sources, absolute recovery of the analytes and the two SAs ranged between 78% and 104% with RSDs not larger than 13%. The accuracy of the method at three different spike levels was assessed by adding the two SAs to analyte-containing milk samples and varied between 82% and 120% with RSDs not larger than 11%. Limits of quantification were estimated to range between 0.008 and 1.4 microg/L. Compared to the Carbograph 4 cartridge, one filled with a N-vinylpyrrolidone-m-divinylbenzene co-polymer (Oasis HLB) sorbent was much less efficient in recovering several of the acidic herbicides considered and, in addition, its relative final extract produced a severe negative matrix effect that drastically weakened ion signal intensities of several non acidic analytes.
Animals↗
Molecularly imprinted polymers grafted to flow through poly(trimethylolpropane trimethacrylate) monoliths for capillary-based solid-phase extraction.
Monolithic molecularly imprinted polymers (mMIPs) have been synthesized in a novel way using a trimethylolpropane trimethacrylate core material photo-polymerized in situ in a 100 microm I.D. UV-transparent capillary and further photo-grafted to create specific cavities in the grafted layer. This polymerization technique allows the imprints to be directly created on the surface of the material using a minimum amount of template. Three different anaesthetics of similar structures (bupivacaine, mepivacaine and S-ropivacaine) were used as model target molecules to synthesize sample enrichment media. Hence, various mMIPs have been prepared and evaluated on a micro-system against each analyte in order to test the retention properties and cross-selectivities of the materials. The retention factors were determined and compared with the non-imprinted reference column (mNIP), yielding high imprinting factors together with good selectivity factors between the three analytes. A study with a pure enantiomeric target was carried out to assess the degree of stereo-specific imprinting for injection of racemic mixtures. Finally, one column was imprinted with an equimolar mixture of all three anaesthetics to provide further comprehension of the retention mechanism and accredit the possibility of using the material as a sample enrichment entity. Scanning electron microscopy (SEM), nitrogen absorption/desorption (BET) and mercury intrusion porosimetry were used to characterize the monolith and the mMIPs properties. Nuclear magnetic resonance (NMR) has been used to assess the similarities between the mMIP and mNIP.
Amides↗
Enantioselective analysis of monoterpenes in different grape varieties during berry ripening using stir bar sorptive extraction- and solid phase extraction-enantioselective-multidimensional gas chromatography-mass spectrometry.
The stereoisomeric ratios of various genuine metabolites of linalool (furanoid and pyranoid linalool oxides, hotrienol) and citronellol (cis- and trans-rose oxide) were determined in grape berries by means of enantioselective-multidimensional gas chromatography-mass spectrometry. Stereoisomers of the metabolites could be separated on a chiral column with a modified cyclodextrin as stationary phase. The detailed stereoselective analysis of the furanoid and pyranoid linalool oxides in the cv. Morio-Muskat during berry ripening is giving evidence that furanoid linalool oxides are generated via two different reaction pathways. Additionally, stereoselective analysis of rose oxide in different varieties that have attained commercial maturity has been performed demonstrating that cis-(2S,4R)-rose oxide is the main stereoisomer in all varieties. (3S)-Hotrienol was the main stereoisomer in all varieties with enantiomeric purities that were always higher than 90%.
Acyclic Monoterpenes↗
Application of solid-phase extraction and liquid chromatography-mass spectrometry to the determination of neonicotinoid pesticide residues in fruit and vegetables.
A rapid and simple method for simultaneous analysis of four neonicotinoid insecticides including acetamiprid, imidacloprid, thiacloprid and thiamethoxam in fruit and vegetable matrices has been developed. For instance, ready-to-use cartridges filled with a macroporous diatomaceous material were used to extract in a single step insecticide residues with dichloromethane from aqueous-acetone extracts of fruits and vegetables. The eluate was evaporated, the residue redissolved with methanol and then analyzed by liquid chromatography-mass spectrometry in the electrospray ionization (ESI) positive mode. Average recoveries of the four pesticides were between 74.5 and 105% at both spiking levels 0.1 and 1.0 mg kg(-1) in peach, pear, courgette, celery and apricot. Relative standard deviations (RSDs) were less than 10% for all of the recovery tests. The calculated limits of quantitation (LOQs) (0.1-0.5 mg kg(-1)) were equal or lower then the maximum residue limits (MRLs) established by European legislation (0.1-0.5 mg kg(-1)). The proposed method is fast, easy to perform and could be utilized for monitoring of pesticides residues.
Chemical Fractionation↗
The isolation and purification of glucoraphanin from broccoli seeds by solid phase extraction and preparative high performance liquid chromatography.
Plant foods contain not only essential nutrients, e.g. protein, amino acids, vitamins and minerals, but also phytochemicals that have added health benefits. One such class of phytochemicals are the glucosinolates. Glucosinolates, particularly glucoraphanin, are predominant in plants of the Brassica genus, most notably in vegetables such as broccoli. There is a growing interest in the role glucoraphanin plays in chemoprotection and as a result there is a requirement to accurately determine the levels of glucoraphanin in vegetable products. Reverse phase ion pair high performance liquid chromatography (HPLC) is the method of choice; however, this work has been hindered by the lack of available standard reference materials. Broccoli seeds, which are particularly rich in glucoraphanin (20-50 mg/g), have proved to be ideal for the isolation of glucoraphanin on the preparative scale. A novel preparative scale HPLC method with simple compound recovery has been developed to meet the need for a glucoraphanin standard.
Brassica↗
Analysis of macrolide antibiotics in river water by solid-phase extraction and liquid chromatography-mass spectrometry.
A liquid chromatography-mass spectrometry (LC-MS) method was developed for the determination of five macrolides in natural water samples, using kitasamycin as surrogate. The macrolides were extracted from water samples using Oasis HLB cartridges. Pre-concentration factors up to 250 were obtained. Separation was carried out in an end-capped silica-based C18 column and mobile phases consisting of water/acetonitrile mixtures containing ammonium acetate. Detection was performed by mass spectrometry with a single quadrupole and a triple quadrupole using an electrospray interface. The quality parameters obtained with these two approaches were compared. The detection limits of the whole process were about 1 ng l(-1). The recoveries from 250 ml of water samples spiked at 25-125 ng l(-1) level were in the range 85-115%, except for azithromycin levels, which were around 70%. Erythromycin-H2O, clarithromycin and azithromyzin were found, at the sub ng l(-1) level, in the studied rivers.
Anti-Bacterial Agents↗
New method for determination of ochratoxin A in beer using zinc acetate and solid-phase extraction silica cartridges.
A new method for the determination of ochratoxin A (OTA) in beer has been developed. The new method has been compared with a reference method currently accepted as AOAC official first action. The limits of detection and quantification of the proposed method were 0.0008 and 0.0025 ng/ml, respectively, while they were 0.0025 and 0.0075 ng/ml, respectively, in the AOAC method used as reference. The recovery levels in the 0.025-0.40 ng OTA/ml spiking range for the proposed and the reference methods were 80.6-87.6% and 78.2-83.8%, respectively. The relative standard deviations of recoveries were 2.6-7.5% for the proposed method and 0.7-6.1% for the reference method. Passing and Bablok regression analysis of recovery data obtained by the proposed method versus data obtained by the reference method on an OTA-spiked beer sample showed good correlation (r2 = 0.9993), while the slope and intercept were 1.049 and -0.0013, respectively. The advantage of the proposed method is the low cost of the materials used in sample preparation because expensive immunoaffinity columns are not needed to clean-up samples while it maintains or even increases the good performance of the reference method. The proposed method was applied to 69 beer samples from different geographic origins (national and imported) but purchased in the Spanish market. They were found to be contaminated with OTA in the range from 0.008 to 0.498 ng/ml (average: 0.070 ng/ml). Five samples surpassed the limit recommended by the European Union (0.2 ng OTA/g).
Beer↗
Retention mechanism of analytes in the solid-phase extraction process using molecularly imprinted polymers. Application to the extraction of triazines from complex matrices.
Two molecularly imprinted polymers (MIPs), prepared in dichloromethane with terbutylazine and ametryn as template molecules, were evaluated for the selective extraction of triazines from complex matrices. Various parameters affecting extraction recoveries on MIPs were studied in order to obtain an optimized extraction procedure allowing to reduce non-specific interactions. In order to test the selectivity of the MIPs, the same procedure was applied to the extraction of compounds possessing the same polarity and size as the triazines. By means of molecular modeling, the effects of the electric charge distribution and of the size of the molecules on the retention mechanism were studied. The value of capacity for terbutylazine MIP was also measured. At last, the high selectivity resulting from the use of MIPs was clearly demonstrated by their applications to the clean-up of grape juice and soil extracts spiked with triazines. In addition, the soil extract was cleaned-up by immunoextraction allowing the comparison of both approaches in terms of selectivity.
Models, Molecular↗
Analysis of PEG 400 and 4000 in urine for gut permeability assessment using solid phase extraction and gel permeation chromatography with refractometric detection.
We developed a treatment of urine samples allowing the analysis of two intestinal permeability markers: polyethylene glycol (PEG) 400 (highly diffusible; basal permeability indicator) and PEG 4000 (poorly diffusible; indicator of an abnormal increase of permeability) by a unique gel permeation chromatography (GPC) with refractometric detection. Urinary PEG were extracted using a mixed-bed resin composed of C2 and C18 layers. Permeability mean values determined in 11 human healthy subjects were 24.20 +/- 9.30% and 0.12 +/- 0.08% for, respectively, PEG 400 and 4000. The percentage of the PEG 4000 permeability value to the one of PEG 400 corresponded to an intestinal permeability index (IPI) of 0.52 +/- 0.35 expressing a low diffusion of this poorly permeability marker.
Adult↗
Quantitation of zidovudine triphosphate concentrations from human peripheral blood mononuclear cells by anion exchange solid phase extraction and liquid chromatography-tandem mass spectroscopy; an indirect quantitation methodology.
To facilitate the assessment of drug safety and determination of phamacokinetics, an anion exchange isolation of zidovudine triphosphate (ZDV-TP) from human peripheral blood mononuclear cells (hPBMC), coupled with dephosphorylation, desaltation, and detection by liquid chromatography-tandem mass spectroscopy (LC-MS-MS) was validated. hPBMCs were harvested from whole blood, lysed, and a suspension of intracellular ZDV-TP was produced. ZDV-TP was isolated from ZDV, ZDV-monophosphate (ZDV-MP), and ZDV-diphosphate (ZDV-DP), which were all present in the cell lysate, by performing a salt gradient anion exchange SPE. Isolated ZDV-TP was dephosphorylated with acid phosphatase to its parent drug form, ZDV. ZDV was then desalted and concentrated for tandem mass spectral detection. An LC-MS-MS methodology was developed and validated for the determination of molar ZDV directly corresponding to the intra-hPBMC molar ZDV-TP concentration. ZDV-TP concentrations were determined in femtomoles per million hPBMCs (fmol/10(6)cells). The assay was able to determine ZDV-TP concentrations accurately and precisely within the range of 5-640 fmol/10(6)cells with 10 million cells per sample analyzed. Inter- and intra-day accuracy and precision data for back calculated standards and quality controls fell within 15% of nominal. The assay correlated well with a previous ELISA method developed and validated in our laboratory, and has been successfully used to quantitate ZDV-TP concentrations in patients being routinely monitored and treated with ZDV.
Chemical Fractionation↗
Determination of eflornithine enantiomers in plasma, by solid-phase extraction and liquid chromatography with evaporative light-scattering detection.
A bioanalytical method for determination of eflornithine (DFMO) in 1000 microL human plasma has been developed and validated. DFMO and the internal standard (IS) were analysed by liquid chromatography with evaporative light-scattering detection (ELSD). Separation was performed on a Chirobiotic TAG (250 mm x 4.6 mm) column with ethanol (99.5%):0.01 mol/L acetic acid-triethylamine buffer at the rate of 25:75% (v/v) with flow rate of 1.0 mL/min. For d-DFMO in plasma the inter-assay precision was 6.5% at 75 micromol/L, 6.6% at 375 micromol/L and 5.8% at 750 micromol/L. For l-DFMO in plasma the inter-assay precision was 10.4% at 75 micromol/L, 6.5% at 375 micromol/L and 5.0% at 750 micromol/L. The lower limit of quantification (LLOQ) was determined to 25 micromol/L where the precision was 4.3% and 5.7%, respectively.
Chromatography, Liquid↗
Determination of captopril in human plasma, using solid phase extraction and high-performance liquid chromatography, coupled to mass spectrometry: application to bioequivalence study.
A specific high performance liquid chromatography-mass spectrometric (LC-MS/MS) assay was developed for the determination of captopryl in plasma. The retention time was 1.45 and 1.37 min for captopril and enalapril, respectively. The overall mean recovery, using SPE extraction with OASIS HLB cartridges, was found to be 107.2+/-9.5 and 100.04+/-2%, respectively. Calibration curves were linear in the concentration range of 10.00-2000.00 ng/ml, and the lower limit of quantification (LLOQ) was 10.00 ng/ml. The LLOQ was sensitive enough for detecting terminal phase concentrations of the drug. Inter-batch precision of the method ranged from 0.88 to 1.95%. Intra-batch accuracy ranged from 97.15 to 105.77%, while intra-batch precision ranged from 2.49 to 5.66% at concentrations of 30.00, 760.00 and 1500.00 ng/ml. The developed method was applied to study bioequivalence of captopril in a group of 25 human subjects at a single oral dose of a 50mg tablet.
Angiotensin-Converting Enzyme Inhibitors↗