Solid-phase Extraction Procedure Research Articles

In situ-floating organic dispersive solid-phase extraction based on putrescine as a new adsorbent for the extraction of ions from crude oil prior to ICP-MS

ABSTRACT Quantification of ions in complex matrices like crude oil is an outstanding issue because of the high complexity of the sample. Herein, a facile, reliable, and precise floating dispersive solid-phase extraction procedure was introduced for the extraction of several ions (B, Ca, Cd, Cu, Cr, Ag, Fe, Mn, Ni, Na, Ba, Mg, Al, Si, Sn, Ti, Mo, V, Pb, Zn, P, and K) in which the need for adding complexing agent for the extraction of ions, centrifugation for separation of adsorbent, and shaker to enhance the contact area of the sample solution with absorbent was eliminated. These advantages were provided by using putrescine as the absorbent for the extraction of the analytes. To reach this goal, a proper amount of putrescine was dissolved in ethanol and injected into a diluted crude oil solution. During this step, putrescine formed stable complexes with the ions and extracted them from the solution and collected on top of the solution easily. The floated phase was collected by a spatula, and the extracted ions were determined by inductively coupled plasma mass spectrometry. Validation parameters of this method showed that low limits of detection (0.003–3.62 ng g−1) and quantification (0.009–12.0 ng g−1), broad linear range (12.0–80,000 ng g−1), acceptable relative standard deviation (≤5.3%) for intra- and inter-day precisions and high extraction recovery (72–90%) were the features of the method. The method was successful in the determination of the analytes in real crude oil samples.

Optimal conditions for determination of bacitracin, bacitracin zinc and bacitracin methylene disalicylate in animal feed by ultra-performance liquid tandem mass spectrometry

An integrated method combining solid-phase extraction (SPE) with ultra-performance liquid tandem mass spectrometry (UPLC-MS/MS) has been established for quantifying bacitracin (BTC), bacitracin zinc (BZ), and bacitracin methylene disalicylate (BMD) in animal feed. A pretreatment procedure that can effectively, quickly, and simultaneously extract and purify BTC, BZ, or BMD in feed was developed for the first time through the optimization of extraction and SPE conditions. After extraction with acetonitrile + methanol + 15 % ammonia solution (1:1:1, v:v:v) and dilution with EDTA solution (1.5 mmol/L, pH 7.0), a SPE procedure was carried out with C18 cartridge. Following LC-MS/MS analysis utilized a Waters Peptide BEH C18 column with a gradient elution of 0.1 % formic acid in water/acetonitrile with. This method demonstrated a strong linear correlation (R2 > 0.9980) across a 0.01–1.0 mg/L concentration span, based on a matrix-matched standard curve. Satisfactory recoveries of BTC (bacitracin A, B1, B2, and B3), BZ, and BMD in different feeds were obtained from 80.7 % to 108.4 %, with relative standard deviations below 15.7 %. Low limits of quantification ranging within 7.2–20 μg/kg were achieved for bacitracin A, B1, B2, and B3. This method provided an effective and reliable detection method to prevent the addition of BTC and different BTC formulations in feeds.

Implementing magnetic molecularly imprinted solid phase extraction to analytical method for determination of 2-phenethylamine in cocoa powder and chocolate by LC-MS/MS system

The main aim of this study was to design, develop, and apply magnetic molecularly imprinted polymer (MMIP) during sample pretreatment before liquid chromatography tandem mass spectrometry (LC-MS/MS) 2-phenylethylamine determination in cocoa powder and chocolate samples. The morphology and structure of MMIP, obtained from methacrylic acid (monomer) and trimethylolpropane trimethacrylate (cross-linker) were characterized using scanning electron microscopy, nitrogen sorption analyses, infra-red spectroscopy, X-ray diffraction measurements, vibrating-sample magnetometry, and thermogravimetry analyses. The analyte adsorption mechanism on MMIP was studied using computational simulation. The magnetic solid phase extraction procedure on MMIP was optimized, resulting in a relative matrix effect of 6.2 % for cocoa powder and 2.8 % for chocolate. The LC-MS/MS quantified the 2-phenethylamine in eighteen cocoa powder and chocolate samples, showing a concentration range between 2.4 and 8.7 μg g−1.

Separation trace amounts of copper ion by solid-phase extraction with carbon-based sorbent prior to flame atomic absorption spectrometry

ABSTRACT In this research, a carbon adsorbent modified with curcumin ligand was utilised in the solid-phase extraction procedure. This method was coupled with flame atomic absorption spectrometry to pre-concentrate and separate trace amounts of copper ions in aqueous solutions. Different experimental parameters, including pH, eluent type and concentration, adsorbent dose, extraction time and sample volume, were studied and optimised. The obtained optimum conditions for the proposed method were: pH of solution, 4.8; extraction time, 9 min; adsorbent dose, 0.01 g; type and concentration of eluent, 1:1 mixture of HCl and HNO3 0.5 mol L−1. Under optimal conditions, the pre-concentration factor of 400.0 and linear range values of the method were 0.031–1.875 µg/L and 12.5–750 µg/L for copper ions in the initial and final solutions, respectively. The relative standard deviation (RSD) for seven replicate detections of 0.05 µg L−1 of copper ion in initial solution was calculated as 2.2%. Furthermore, the detection limit of 0.008 µg L−1 was determined for the suggested method. In order to investigate the selectivity of modified carbon adsorbent, the influence of some interfering ions on the extraction and recovery of Cu (II) was studied. Finally, the present method was employed for the determination of copper ions in real water samples and standard alloys.

Simultaneous Determination of 17 Phenolic Compounds in Surface Water and Wastewater Matrices Using an HPLC-DAD Method

A high-performance liquid chromatography with diode array detector (HPLC-DAD) analytical method was developed for the simultaneous detection of 17 phenolic compounds, including phenols, chlorophenols, alkylphenols, and nitrophenols, in two types of water matrices: wastewater and surface water. Prior to HPLC-DAD determination, a solid-phase extraction (SPE) procedure was optimized. The proposed method uses multiwavelength analysis, with the optimum detection wavelengths selected as 268 nm, 280 nm, 386 nm, 304 nm, and 316 nm. The highest resolution was achieved using a chromatographic column, Eclipse XDB-C18 (150 × 4.6 mm, 5 μm), which was kept at 20 °C. The mobile phase consisted of a gradient elution program, with mobile phase A being a 0.1% H3PO4 aqueous solution and mobile phase B being acetonitrile. The flow rate was set at 0.6 mL/min. The 17 target phenolic compounds were fully separated in less than 27 min. All compounds showed good linear regression, with correlation coefficients higher than 0.999. The method’s quantitation limits ranged from 4.38 to 89.7 ng/L for surface water and 7.83 to 167 ng/L for wastewater. The recovery rates were in the range of 86.2–95.1% for surface water and 79.1–86.3% for wastewater. The SPE-HPLC-DAD method was proven to be fast, sensitive, accurate, and reproducible. The developed method was successfully applied for the analysis of the 17 phenolic compounds in real surface water and wastewater samples, with phenol, 2,4-DNP, and 2,4-DNP being determined at levels greater than the method’s limits of quantitation (LOQs). The proposed analytical method represents an original technical resource for the simultaneous determination of 17 phenolic compounds in environmental water matrices.

Analytical control of imatinib in bioanalytical samples using graphene quantum dots sensing.

An analytical method for the determination of imatinib (IMA, the primary treatment for chronic myeloid leukemia), based on the fluorescence properties of graphene quantum dots (GQDs), is reported in this work. The method is addressed to the analytical control of IMA in biological and pharmaceutical samples, due to the present interest in the control of the doses of this anticancer drug, as well as the therapeutic monitoring. The whole method involves the use of a solid-phase extraction (SPE) procedure, followed by an evaporation step, for the treatment of biological samples. For that, tC18 sorbent cartridges were used. After the sample treatment, the solution containing the analyte was mixed with an aqueous solution of GQDs at pH 7.2, and the fluorescent quenching of GQDs was measured. IMA was determined in the 10-250µgL-1 range, with a limit of detection of 21µgL-1 and a precision of 1.5% as relative standard deviation, measured in terms of reproducibility. The recovery for biological samples was in the 84-113% range.

Amanitin determination in bile samples by UHPLC-MS: LR-MS and HR-MS analytical performance

Consumption of misidentified foraged mushrooms containing bicyclic amanitin octapeptides is a worldwide public health and veterinary problem, being considered one of the deadliest accidental human and canine food ingestion due to acute liver failure (ALF). Reversal of advanced ALF and complete clinical recovery can be achieved following definitive removal of accumulated amatoxin laden bile from the gallbladder. An accurate means of quantifying amanitin content in aspirated bile is, therefore, urgently needed. Building on our prior work validating a method to detect and quantify amanitin in hepatic autopsy tissue, the development of an accurate method of measuring α- and β-amanitin in aspirated gallbladder bile was performed to evaluate the efficiency of this emergency procedure applied as a clinical treatment for intoxicated patients. A solid-phase extraction (SPE) procedure was optimized followed by detection based on ultra-high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS). Low resolution mass spectrometry (LRMS) was compared with high resolution (HRMS) by the validation of UHPLC-MS/MS (triple quadrupole MS) and UHPLC-ToF-MS (time-of-flight MS). Both methods were able to detect amatoxins in bile with limits of detection and quantification ranging from 2.71 to 3.46 µg.kg-1, and 8.36–9.03 µg.kg-1 for α-amanitin and, 0.32–1.69 µg.kg-1 and 0.55–5.62 µg.kg-1 for β-amanitin, respectively. Validation was completed with the evaluation of linearity, specificity, robustness, recovery, and precision following the ICH guidelines and CIR 808/2021. The validated methods were finally applied to bile samples obtained 48–96 hours + post-ingestion from 4 amatoxin poisoning patients who underwent gallbladder drainage procedures in Vietnam, Canada, and California. Gallbladder bile from patients with amatoxin mushroom poisoning contained significant amanitin content, even when aspirated several days post-ingestion, thus confirming the important role of enterohepatic circulation in amatoxin hepatotoxicity. This work represents a high and unique analytical throughput in amanitin poisoning allowing to efficiently respond to this fatal health problem.

Trace analysis of 20 antihistamines in milk by ultrahigh performance liquid chromatography coupled with high field quadrupole orbitrap high resolution mass spectrometry followed dispersive micro solid phase extraction

Ultrahigh-performance liquid chromatography coupled with high-field quadrupole Orbitrap high resolution mass spectrometry was used for the separation and determination of 20 antihistamines, and a dispersive micro solid-phase extraction procedure using high-performance absorbing material was developed as a sample preparation strategy for extracting 20 antihistamines from milk. Instrument conditions and key parameters influencing extraction efficiency were investigated to obtain an optimized method. The limit of detection for 20 antihistamines in milk using this method is 0.05 µg/L to 1.0 µg/L. Recoveries are between 80.7 % and 108.3 %, and the relative standard deviation is less than 15 %. It is suitable for confirmatory monitoring and quantitative analysis of 20 antihistamines in milk. The results show that antihistamines in milk may be noteworthy issues for human health and environmental pollution.

Validation of an efficient analytical method for quantification of tetracycline antibiotic residues in egg samples along with investigating their decontamination using ultraviolet waves

ABSTRACT This study describes the development and application of a dispersive solid-phase extraction procedure combined with dispersive liquid – liquid microextraction for the extraction of tetracycline antibiotics from egg samples. In this method, a bio-metal organic framework was prepared and used in extraction of the analytes from sample solution. In this method, the sorbent synthesis was relatively easy and its crosslinker was vitamin B3 which is a green chemical compound. The sorbent provides particles can extract the analytes via interactions such as surface adsorption, occlusion van der waals and π–π interactions. The extraction procedure was done by mixing trichloroacetic acid with the egg sample to remove the sample proteins and then the synthesised sorbent at mg – level was added to the supernatant phase and the mixture was vortexed. After centrifuging, the supernatant phase was removed and sorbent particles containing the extracted analytes were eluted using acetonitrile. After that, this phase containing the analytes was taken and used in the following dispersive liquid – liquid microextraction process that was done to more enrichment the analytes using a deep eutectic solvent. After optimisation of the extraction process, sensitive limits of detection and quantification were found in the ranges of 0.21–0.28 and 0.70–0.93 ng g−1, respectively. Acceptable extraction recoveries of the analytes ranged from 60 to 73%. The method was selective regarding the analytes, as there were no interfering peaks eluted at the retention times of the analytes. After the validation step, the offered method was employed for the determination of the tetracycline antibiotics in various egg samples and the effect of ultraviolet waves in decontaminating them from egg samples was investigated.

Preconcentration and Removal of Lead From Water Samples Using Magnetic Copper Ferrite Nanoparticles

The presence of lead and its compounds is extremely dangerous to various forms of life. Therefore, exploring effective treatments that can reduce the presence of lead ions around us becomes crucial, thereby averting lead toxicity. A magnetic solid phase extraction (MSPE) procedure for the removal and preconcentration of trace amounts of Pb(II) using copper ferrite nanoparticles (CuFe2O4 NPs) prior to their determination by flame atomic absorption spectrometry (FAAS) has been proposed. CuFe2O4 as solid-phase extraction adsorbent was synthesized via co-precipitation and characterized by attenuated total reflection–infrared spectroscopy (ATR–IR), x-ray diffraction spectrometry (XRD), and scanning electron microscopy (SEM). These magnetic CuFe2O4 carrying the Pb(II) could be easily separated from the aqueous solution by applying an external magnetic field; no filtration or centrifugation was necessary. Various analytical parameters, including pH, eluent type/concentration, adsorbent mass, sample volume, adsorption/desorption time, mixing, and interfering ions, were systematically studied and optimized for the recovery of Pb(II). A sample volume of 20 mL achieved a preconcentration factor of 20. The method effectively determined Pb(II) in water samples, with recovery values exceeding 95% using the optimal conditions.

DEVELOPMENT AND VALIDATION OF AN LC-MS/MS METHOD FOR THE DETERMINATION OF TENOFOVIR AND EMTRICITABINE

Objective: Therapeutic drug monitoring of tenofovir and emtricitabine, two commonly used antiretroviral drugs, is important to maximize effectiveness while minimizing side effects. Materials: A Liquid Chromatography-Mass spectrometry (LC-MS/MS) method was developed to quantify tenofovir and emtricitabine in human plasma samples. The method involves a simple solid phase extraction procedure followed by liquid chromatography separation using a Penta Fluoro Phenyl (PFP) column with a Phenomenex C18 column and a mobile phase of ammonium formate, acetonitrile, and methanol, achieving separation in under 4 min. Results: The method showed good accuracy, low limits of quantification, adequate recovery, minimal matrix effects, and specificity. Analyte stability under multiple storage conditions was demonstrated. Conclusion: The validated LC-MS/MS method provides a reliable tool for therapeutic drug monitoring and pharmacokinetic studies of anti-Human Immuno-deficiency Virus (HIV) regimens. The assay can be applied to large populations, especially in resource-poor settings, to help individualize dosing and improve clinical outcomes while reducing toxicity.

Use of the dummy approach for the synthesis of ion imprinted polymers with Ni(II) or Zn(II) as template ion for the solid-phase extraction of Cu(II).

There is a strong interest in monitoring copper in environmental waters, but its direct analysis suffers from strong matrix interferences. This is why, a sample pretreatment based on solid-phase extraction (SPE) is often used but conventional sorbents usually lack specificity. It is overcome with ion-imprinted polymers (IIPs). This work evaluates for the first time the use of the dummy approach for the synthesis of Cu(II)-targeting IIPs. Two analog ions Ni(II) and Zn(II) were tested as templates and the resulting IIPs were packed in SPE cartridges. The SPE procedure was designed by optimizing a washing step following the sample percolation, to eliminate the interfering ions retained on the IIP by non-specific interactions. To optimize the washing step, solutions at different pH or containing tris(hydroxymethyl)aminomethane as a complexing agent at different concentrations were tested and combined. Zn-IIP appeared more promising than Ni-IIP, showing excellent specificity and a high selectivity. Its retention capacity was determined to be 100µg/g, and different isotherm models were evaluated to fit with the adsorption data. Finally, applications to mineral and sea waters were successfully completed and led to high and repeatable extraction recoveries for Cu(II) (88±1% and 83±3%, respectively).

Dietary Risk Assessment of Cyromazine and Its Analogue Melamine in Evaporated and Infant Milk Samples in Nigeria

Background: The safety of milk is considered as a significant public health consideration and has been a key concern for consumers worldwide. The concentrations of cyromazine and its metabolic product, melamine, and their dietary risk assessment are investigated in this study.
 Methods: A total of 182 milk samples containing 15 brands were sampled between June and December 2022 from major and retail markets in Nigeria. After a solid-phase extraction procedure, the concentrations of the two compounds were determined using High-Performance Liquid Chromatography coupled with a Diode-Array Detector. Solid-phase extraction was utilized to extract local and imported evaporated and infant milk with CCl3COOH and CH3CN, followed by clean-up with NH4OH in MeOH. The extracts were analyzed with Agilent High-Performance Liquid Chromatography, including a Zorbax Eclipse+C18 column.
 Results: For both melamine and cyromazine, the Limits of Detection and Limits of Quantification were 1.29-1.48 and 3.94-4.50 µg/kg, respectively. The precision (Relative Standard Deviation<1), recovery (99.5–102.5%), and regression (r2=0.989) were all excellent. Melamine concentration ranged between 57.6±18.9 and 930.3±379.9 µg/kg among the samples, and cyromazine was 57.2±12.3 and 670.9±87.8 µg/kg. Brand 2, imported from Holland, had the highest detection frequency for the two analytes. Disturbing levels of melamine were detected in Brand 2, particularly that 75 and 95% of the samples had melamine above the acceptable Maximum Residue Limit. However, the estimated daily exposure to the two additives was below the allowed daily intake values, and the Hazard Index (HI) in the different milk samples ranged from 0.02 to 1.22, with one sample having HI>1.
 Conclusion: The exposure risk of melamine and cyromazine among the general population is acceptable, and smaller HI values demonstrated no significant potential risk for the Nigerian population according to the recommended guidelines. Regulatory agencies are encouraged to step up their surveillance activities to forestall the inclusion of prohibited additives in local and imported milk to protect public health.

Capillary electrophoresis tandem mass spectrometry to determine multiclass cyanotoxins in reservoir water and spinach samples

Cyanotoxins constitute a group of toxic secondary metabolites, the presence of which in any water body poses a major health risk. Moreover, advanced organisms such as edible plants exposed to these toxins, are a possible pathway for human exposure. Green analytical chemistry is demanding environmentally friendly analytical techniques. In this sense, we propose the use of capillary electrophoresis coupled to tandem mass spectrometry (CE-MS/MS) to determine a mixture of eight cyanotoxins belonging to three different classes: cyclic peptides (microcystin-LR, microcystin-RR and nodularin), alkaloids (cylindrospermopsin and anatoxin-a) and three isomeric non-protein amino acids (β-methylamino-l-alanine, 2,4-diaminobutyric acid and N-(2-aminoethyl)glycine). Separation was achieved by using an acidic background electrolyte consisting of 2 M formic acid and 20% acetonitrile in water. Parameters affecting MS/MS detection and the sheath-liquid interface were also studied. Finally, a combination of pH-junction, field-amplified sample stacking (FASS) and acid barrage as online preconcentration strategies, was employed to improve sensitivity and efficiency. The online preconcentration applied, in combination with a dual cartridge solid-phase extraction (SPE) system, allows to obtain limits of detection in the very low range of µg·L−1 for these multiclass cyanotoxins in reservoir water samples (from 0.005 to 0.10 µg·L−1). Furthermore, for the first time cyanotoxins are analysed in spinach samples through CE-MS/MS using the same SPE procedure, following lyophilisation and solid-liquid extraction with 6 mL 80 % aqueous MeOH.

Analysis of 14 β-agonists in pork using an automated wooden tip-based solid-phase microextraction device and ultra-high-performance liquid chromatography-tandem mass spectrometry.

This study introduces a cost-effective, automated ultra-high-performance liquid chromatography-tandem mass spectrometry method for the detection of 14 β-agonists in pork using a novel solid-phase microextraction probe composed of polyacrylonitrile and molecularly imprinted polymer. Integrated into an automated extraction device, the probe optimizes extraction prior to analysis while reducing expenses and time compared to traditional solid-phase extraction procedures. The method validation followed the Chinese National Standard (GB/T 27404-2008) and examined limits of detection, limits of quantification, matrix effects, linearity, intraday, and interday precision. Average recovery rates ranged from 71.6% to 82.2%, with relative standard deviations less than 15%. Limits of detection and limits of quantification ranged from 0.09 to 0.39 and 0.27 to 0.99μg/kg, respectively. The new method identified positive samples more accurately than the current National Standard GB/T 31658.22-2022 and demonstrated its potential for routine assessment and regulatory compliance in the detection of β-agonists in pork.

Novel advanced materials and magnetic solid phase extraction as approaches in sample preparation to enhance the analysis of ochratoxin A in peanuts.

Ochratoxin A (OTA) is a mycotoxin that can contaminate a variety of agricultural commodities, including fruit juices and wines. The capability of a magnetic solid-phase extraction (MSPE) method with a magnetic metal-organic framework (MOF) material having a three-layer core-shell structure to improve the detection of OTA in food matrices using high performance liquid chromatography is described. Analysis of the material through X-ray diffraction (XRD) indicated the successful synthesis of the magnetic nanomaterial Fe3O4@SiO2@UiO66-NH2. Scanning electron microscopy (SEM) and Zetasizer lab indicated its nano-sized morphological features. The conditions affecting the magnetic solid-phase extraction procedure, such as material dosage, pH, composition and amount of eluent, desorption solution and desorption time were investigated to obtain the optimal extraction conditions. Under optimized conditions, the recoveries of spiked analytes at three different concentrations ranged from 95.83 to 101.5%, and the relative standard deviations were below 5%. Coupling with HPLC allowed the limit of detection to be 0.3 μg kg-1. This method is simple and specific, and can effectively avoid the influence of coexisting elements and improve the sensitivity of determination through fast MSPE of OTA. It has broad development prospects in OTA detection pre-treatment.

Polymeric Materials in Speciation Analysis Based on Solid-Phase Extraction.

Speciation analysis is a relevant topic since the (eco)toxicity, bioavailability, bio (geo)chemical cycles, and mobility of a given element depend on its chemical forms (oxidation state, organic ligands, etc.). The reliability of analytical results for chemical species of elements depends mostly on the maintaining of their stability during the sample pretreatment step and on the selectivity of further separation step. Solid-phase extraction (SPE) is a matter of choice as the most suitable and widely used procedure for both enrichment of chemical species of elements and their separation. The features of sorbent material are of great importance to ensure extraction efficiency from one side and selectivity from the other side of the SPE procedure. This review presents an update on the application of polymeric materials in solid-phase extraction used in nonchromatographic methods for speciation analysis.

Dispersive solid phase extraction of tacrolimus from biological samples using curcumin and iron-based metal organic frameworks nanocomposite followed by LC-MS/MS determination

Tacrolimus is a potent immunosuppressive drug used in the prevention of tissue rejection. It has a narrow therapeutic index. Therefore, the determination of its concentration in biological fluids like plasma and urine is a very crucial issue. In this research, tacrolimus concentrations in plasma and urine samples were determined with a dispersive solid phase extraction procedure coupled to high-performance liquid chromatography-tandem mass spectrometry. For this purpose, a curcumin modified metal-organic framework was synthesized and used in extraction procedure. Tacrolimus was adsorbed onto the sorbent surface with aid of vortexing. Then, the adsorbed tacrolimus was eluted by a suitable solvent. Important parameters in extraction procedure were optimized by “one-variable-at-a-time” approach and reported as below: sorbent amount, 10 mg; sample solution pH, 2; agitation mode, vortexing; adsorption and desorption times, 1 min, and eluent (volume), methanol (200 µL). Under the optimized conditions and according to the International Council for Harmonization guidelines, the validation of the method was performed, and the results showed acceptable accuracy and precision (relative standard deviations ≤14 %), good linearity in a wide range (4–200 ng mL−1), and low limits of detection (1.2 ng mL−1 in plasma and 0.34 ng mL−1 in urine) and quantification (4.7 ng mL−1 in plasma and 1.12 ng mL−1 in urine). Finally, the validated method was successfully applied for the determination of tacrolimus in the plasma samples of the patients.

Evaluation of solid-phase extraction sorbents for purification of oligosaccharides and glycans derivatized by positively charged labels followed by capillary electrophoretic analysis.

The sample preparation including labeling and clean-up represents a key analytical step in the analysis of oligosaccharides and glycans by either chromatographic or electrophoretic separation methods. Although the majority of labeling has been performed by neutral and/or negatively charged tags, the introduction of a positive charge into the saccharide molecule can significantly improve the analysis, especially with mass spectrometry detection. In this work, we present the evaluation of five solid-phase extraction sorbents differing in extraction chemistry for the clean-up and concentration of positively labeled maltooligosaccharides from the reaction mixtures. Maltooligosaccharides containing four to seven glucose units were labeled by cationic tags (2-aminoethyl)trimethylammonium chloride and (carboxymethyl)trimethylammonium chloride hydrazide and the extraction conditions were optimized followed by electrophoretic analysis with conductivity detection. The effects of the solid-phase extraction sorbent chemistry, extraction conditions, and sample composition are discussed. All tested sorbents were capable of cleaning up maltooligosaccharides from the reaction mixtures to some extent after optimization of the solid-phase extraction procedure (51.9%-98.9% recovery). The best-rated amide-based sorbent was used to process the sample of N-linked glycans enzymatically released from ribonuclease B.

A magnetic solid phase extraction procedure for Pb(II) at trace levels on magnetic Luffa@TiO2 in food and water samples.

A novel magnetic Luffa@TiO2 sorbent was synthesized and characterized by using XRD, FTIR and SEM techniques. Magnetic Luffa@TiO2 was used for solid phase extraction of Pb(II) in food and water samples prior to its flame atomic absorption spectrometric (FAAS) detection. The analytical parameters such as pH, adsorbent quantity, type and volume of eluent, and foreign ions were optimized. Analytical features such as the limit of detection (LOD) and the limit of quantification (LOQ) of Pb(II) are 0.04μg L-1 and 0.13μg L-1 for liquid samples and 0.159ng/g and 0.529ng/g for solid samples, respectively. The preconcentration factor (PF) and relative standard deviation (RSD%) were found 50, and 4 % respectively. The method was validated by using three certified reference materials (NIST SRM 1577b bovine liver, TMDA-53.3 and TMDA-64.3fortified water). The presented method was applied to lead contents of some food and natural water samples.