Relative Detection Limits Research Articles

Synthesis of L-tyrosine-capped ZnSe quantum dots and its application to hypochlorite determination in water

ABSTRACTIn this study, a new sensitised spectrofluorometric method was presented as a probe sensor for hypochlorite analysis in oral and tap water samples. By capping L-tyrosine (Tyr) on ZnSe nanoparticles, stable quantum dots (QDs) were obtained. In comparison with Tyr, the fluorescence (FL) emission of Tyr-capped ZnSe is enhanced and shifted to greater wavelength, which causes to enhance the sensitivity for the determination of hypochlorite. Based on the FL quenching of the Tyr-capped ZnSe QDs, hypochlorite concentration was detected at buffering pH of 7 in the range of 5.15 × 10−5‒2.57 × 10−2 g L−1. Relative standard deviation and detection limit were found to be 0.83% and 2.06 × 10−5 g L−1, respectively. In comparison with the other methods of hypochlorite determination, this method is simple, fast and inexpensive, with low sample volume consumption. It also exhibits a good selectivity.

Development of a microfluidic-chip system for liquid–phase microextraction based on two immiscible organic solvents for the extraction and preconcentration of some hormonal drugs

In the present study, for the first time, an on-chip liquid phase microextraction (LPME) coupled with high performance liquid chromatography was introduced for the analysis of levonorgestrel (Levo), dydrogesterone (Dydo) and medroxyprogesterone (Medo) as the model analytes in biological samples. The chip-based LPME set-up was composed of two polymethyl methacrylate (PMMA) plates with microfabricated channels and a microporous membrane sandwiched between them to separate the sample solution and acceptor phase. These channels were used as a flow path for the sample solution and a thin compartment for the acceptor phase, respectively. In this system, two immiscible organic solvents were used as supported liquid membrane (SLM) and acceptor phase, respectively. During extraction, the model analytes in the sample solution were transported through the SLM (n-dodecane) into the acceptor organic solvent (methanol). The new set-up provided effective and reproducible extractions using low volumes of the sample solution. The effective parameters on the extraction efficiency of the model analytes were optimized using one variable at a time method. Under the optimized conditions, the new set-up provided good linearity in the range of 5.0–500µgL−1 for the model analytes with the coefficients of determination (r2) higher than 0.9909. The relative standard deviations (RSDs%) and limits of detection (LODs) values were less than 6.5% (n=5) and 5.0µgL−1, respectively. The preconcentration factors (PFs) were obtained using 1.0mL of the sample solution and 20.0µL of the acceptor solution higher than 19.9-fold. Finally, the proposed method was successfully applied for the extraction and determination of the model analytes in urine samples.

Preparation of a K(+) -imprinted polymer for the selective recognition of K(+) in food samples.

An analytical method is reported for the preparation of K(+) -imprinted nanoparticles using cryptand 222 as the complexing agent, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the crosslinker and 2,2'-azobisisobutyronitrile as the radical initiator. The prepared particles have a diameter of 200-250 nm. The maximum adsorption capacity of potassium ion-imprinted polymer particles was 120 μmol/g. The optimum pH for quantitative extraction was 9.0. The nature of the eluent, eluent concentration, adsorption and desorption times, weight of the polymer material, aqueous phase, and desorption volumes were also studied. The relative selectivity coefficients of K(+) /Li(+) , K(+) /Na(+) , K(+) /Rb(+) and K(+) /Cs(+) were 48.10, 4.80, 29.70, and 43.4, respectively. The relative standard deviation and limit of detection of the method were obtained 1.61% and 4.62 ng/L, respectively. Finally, the method was applied for the determination of potassium ions from different samples using flame photometry.

Determination of emerging nitrogenous economic adulterants in milk proteins by high-performance liquid chromatography/compact mass spectrometry.

Milk-derived ingredients are widely used around the world in the manufacturing of nutritional products. They are prone to economically motivated adulteration with nitrogenous compounds such as melamine and its analogs in order to increase the nitrogen content of these ingredients. The need to rapidly screen milk-derived ingredients to detect adulteration is of paramount public health concern. A liquid chromatography/mass spectrometry (LC/MS)-based method using a single quadrupole mass spectrometer has been developed for the rapid frontline analysis of six nitrogenous protein adulterants, i.e. melamine, ammeline, ammelide, amidinourea, cyromazine and cyanuric acid, in three key milk-derived ingredients, i.e. whole milk powder, nonfat milk powder and whey protein concentrate. The sample preparation scheme involves both 'dilute and shoot' as well as solid-phase extraction (SPE)-based methods. The 'dilute and shoot' scheme uses a tenfold dilution of sample with water followed by protein precipitation using 2% formic acid in acetonitrile. The SPE scheme involves tenfold dilution of sample with water, followed by protein precipitation using acetonitrile, and further cleanup through Strata Melamine SPE cartridges. Sample extracts were analyzed by hydrophilic interaction chromatography/single quadrupole mass spectrometry (HILIC/MS) in both positive and negative electrospray ionization mode. Accurate quantitation was achieved using stable isotope labeled internal standards. A multi-day method validation study was conducted using three different milk-derived ingredients. Average accuracies, relative standard deviations (RSD) and method detection limits (MDL) for all analytes in whole milk powder were 65-118%, 7-11% and 0.9-30 mg/kg, using the 'dilute and shoot' extraction procedure. The SPE procedure results were 102-111%, 5-13%, and 0.4-2.5 mg/kg, respectively, for melamine, ammeline, ammelide and cyromazine only. A rugged and simple to use analytical method to screen for the presence of nitrogenous economic adulterants in milk-derived ingredients has been developed for routine frontline use. Copyright © 2016 John Wiley & Sons, Ltd.

Tailor-made ion-imprinted polymer based on functionalized graphene oxide for the preconcentration and determination of trace copper in food samples.

A tailor-made Cu(II) ion-imprinted polymer based on large-surface-area graphene oxide sheets has been synthesized for the preconcentration and determination of trace copper from food samples by solid-phase extraction. Attributed to the ultrahigh surface area and hydrophilicity of graphene oxide, the Cu(II) ion-imprinted polymer prepared by the surface ion-imprinting technique exhibited a high binding capacity and a fast adsorption rate under the optimized experimental conditions. In the static adsorption experiments, the maximum adsorption capacity of Cu(II) ion-imprinted polymer is 109.38 mg/g at 25°C, which is much higher than that of the nonimprinted polymer (32.12 mg/g). Meanwhile, the adsorption is very rapid and equilibrium is reached after approximately 30 min. The adsorption mechanism is found to follow Langmuir adsorption model and the pseudo-second-order adsorption process. The Cu(II) ion-imprinted polymer was used for extracting and detecting Cu(II) in food samples combined with graphite flame atomic adsorption spectrometry with high recoveries in the range of 97.6-103.3%. The relative standard deviation and limit of detection of the method were evaluated as 1.2% and 0.37 μg/L, respectively. The results showed that the novel absorbent can be utilized as an effective material for the selective enrichment and determination of Cu(II) from food samples.

Ru(bpy)3(2+)/nanoporous silver-based electrochemiluminescence immunosensor for alpha fetoprotein enhanced by gold nanoparticles decorated black carbon intercalated reduced graphene oxide.

A highly sensitive sandwich-type electrochemiluminescence (ECL) immunosensor was proposed for the quantitative determination of alpha fetoprotein (AFP) using gold nanoparticles decorated black carbon intercalated reduced graphene oxide (Au-rGO@CB) as sensing platform and nanoporous silver (NPS) loaded Ru(bpy)32+ as labels. In this work, intercalation of CB inhibited the accumulation of rGO and Au-rGO@CB was firstly used to immobilize primary antibody (Ab1) in ECL system. NPS prepared by the dealloying of binary alloy has high pore volume and surface areas, which was used to load amount of secondary antibodies (Ab2) and Ru(bpy)32+, which could greatly enhance the ECL intensity. Under optimal conditions, the designed immunosensor exhibited wider linear range from 0.0001 to 30 ng/mL with a relative lower detection limit of 33 fg/mL for AFP detection. Overall, the designed immunosensor exhibited high sensitivity and selectivity, good repeatability and stability. This proposed method provided a potential application for clinical monitoring of AFP.

A Rapid and Cost‐Efficient Technique for Simultaneous/Duplex Detection of Listeria Monocytogenes and Escherichia Coli O157:H7 Using Real Time PCR

AbstractThe increasing industrial interest in easy, economical and reliable methods has led to the development and application of DNA‐based methods for the detection of microbial pathogens in food. In the present article, we describe the development of a cost‐efficient EvaGreen‐based real‐time Polymerase chain reaction (PCR) technique for simultaneous and practical detection of Listeria monocytogenes (L. monocytogenes) and Escherichia coli O157:H7 (E. coli O157:H7) in the food matrix. EvaGreen‐based simplex and duplex real‐time PCR showed that specific PCR products were identified by melting curve analysis, and had a reproducible Tm of 77.00 ± 0.4C for L. monocytogenes and 85.60 ± 0.2 for E. coli O157:H7.The absolute detection limit of Eva Green‐based simplex and duplex real‐time PCR was 0.0001 ng/μL for DNA of both pathogens. The relative detection limit of the simplex and duplex technique was less than 10 cells/mL for the two pathogens.Practical ApplicationsThis study illustrates a rapid, effective and cheap identification method to simultaneously monitor two foodborne pathogens in food samples. The specificity and sensitivity of this method can be used to clearly identify these two foodborne pathogens in practical food samples based on the specific genes of the species. Hence, this detection method is applicable to surveillance measures for these two foodborne pathogens in the food production chain. Moreover, this technique is used by food control laboratories in a secure way.

Indirect chiral separation of tryptophan enantiomers by high performance liquid chromatography with indirect chemiluminiscence detection.

In recent years, the study of chiral compounds in vivo has received much attention. In this study, a novel method based on high performance liquid chromatography (HPLC) coupled with chemiluminescence (CL) detection was developed for the separation of tryptophan (Trp) enantiomers. o-Phthalaldehyde and N-acetyl-l-cysteine were used as chiral derivatization reagents for Trp before it can be detected by HPLC-CL method. The separation was carried out on an ODS column using a mobile phase composed of methanol-0.01mol/L phosphate buffer (40/60, v/v). Under the optimum conditions, satisfactory results were obtained, including complete separation, good relative standard deviations and low detection limits. The applicability of the proposed method has been validated by determining Trp in biological samples. Linear responses (r>0.9990) were observed over the range of 2.5×10(-7) to 1.2×10(-5)g/mL of Trp enantiomers, with quantitation limit of 2.5×10(-7)g/mL. The assay method shows good specificity to Trp enantiomers, and thus it will have great potential application in clinical diagnosis. The mean extraction efficiency of Trp enantiomers in mice plasma samples were 98.48% and 97.40%, respectively. The mean relative standard deviation (RSD) of Trp enantiomers were <3%.

A new magnetic ion-imprinted polymer as a highly selective sorbent for determination of cobalt in biological and environmental samples

A magnetic ion-imprinted polymer (Fe3O4@TiO2@SiO2-IIP) functionalized with -NH groups for the selective determination of Co(II) ions from environmental and biological samples is presented. This sorbent was synthesized by surface imprinting technique combined with sol-gel process using 3-(2-aminoethylamino) propyltrimethoxysilane (AAPTS) as a functional ligand, tetraethyl orthosilicate as across-linking agent, and Co(II) ion as the template. The prepared magnetic ion-imprinted polymer was characterized by infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), dynamic light scattering (DLS), and X-ray diffraction (XRD). Fe3O4@TiO2@SiO2-IIP showed higher capacity and selectivity than that of Fe3O4@TiO2@SiO2-NIP. The important parameters influencing the recovery such as pH, the volume and eluent concentration, contact time, and the amount of sorbent on extraction percentage of Fe3O4@TiO2@SiO2-IIP were studied and optimized. The linear range (LR), relative standard deviation(RSD) and limit of detection (LOD=3 S(b)/m) for flame atomic absorption spectrometric determination of Co(II) ion, after its selective extraction by the prepared IIP polymer, were evaluated as 1-130 µg L(-1), 1.22% and 0.15 µg L(-1), respectively. The maximum capacity of Fe3O4@TiO2@SiO2-IIP and Fe3O4@TiO2@SiO2-NIP is 35.21 mg g(-1) and 10.34 mg g(-1), respectively. The separation factor of Fe3O4@TiO2@SiO2-IIP for Co(II)/Pb(II), Co(II)/Ni(II), and Co(II)/Cd(II) are 41.17, 79.74, and 56.48, respectively. In addition, the spent magnetic ion-imprinted polymer can be refreshed by simply washing with an aqueous HNO3 solution, and there is no significant decrease in adsorption capacity after a test of upto seven cycles, demonstrating that the Fe3O4@ TiO2@SiO2-IIP is stable and reusable.

A new specific reference gene based on growth hormone gene (GH1) used for detection and relative quantification of Aquadvantage® GM salmon (Salmo salar L.) in food products

Genetic transformation of fish is mainly oriented towards the improvement of growth for the benefit of the aquaculture. Actually, Atlantic salmon (Salmo salar) is the species most transformed to achieve growth rates quite large compared to the wild. To anticipate the presence of contaminations with GM salmon in fish markets and the lack of labeling regulations with a mandatory threshold, the proper methods are needed to test the authenticity of the ingredients. A quantitative real-time polymerase chain reaction (QRT-PCR) method was used in this study. Ct values were obtained and validated using 15 processed food containing salmon. The relative and absolute limits of detection were 0.01% and 0.01ng/μl of genomic DNA, respectively. Results demonstrate that the developed QRT-PCR method is suitable specifically for identification of S. salar in food ingredients based on the salmon growth hormone gene 1 (GH1). The processes used to develop the specific salmon reference gene case study are intended to serve as a model for performing quantification of Aquadvantage® GM salmon on future genetically modified (GM) fish to be commercialized.

Amplified solid-state electrochemiluminescence detection of cholesterol in near-infrared range based on CdTe quantum dots decorated multiwalled carbon nanotubes@reduced graphene oxide nanoribbons

An amplified solid-state electrochemiluminescence (ECL) biosensor for detection of cholesterol in near-infrared (NIR) range was constructed based on CdTe quantum dots (QDs) decorated multiwalled carbon nanotubes@reduced graphene nanoribbons (CdTe-MWCNTs@rGONRs), which were prepared by electrostatic interactions. The CdTe QDs decorated on the MWCNTs@rGONRs resulted in the amplified ECL intensity by ~4.5 fold and decreased onset potential by ~100 mV. By immobilization of the cholesterol oxidase (ChOx) and NIR CdTe-MWCNTs@rGONRs on the electrode surface, a solid-state ECL biosensor for cholesterol detection was constructed. When cholesterol was added to the detection solution, the immobilized ChOx catalyzed the oxidation of cholesterol to generate H2O2, which could be used as the co-reactant in the ECL system of CdTe-MWCNTs@rGONRs. The as-prepared biosensor exhibited good performance for cholesterol detection including good reproducibility, selectivity, and acceptable linear range from 1 μM to 1mM with a relative low detection limit of 0.33 μM (S/N=3). The biosensor was successfully applied to the determination of cholesterol in biological fluid and food sample, which would open a new possibility for development of solid-state ECL biosensors with NIR emitters.

Comparison and evaluation of two methods for the pesticide residue analysis of organophosphates in yerba mate

Microwave Assisted Extraction and a modified CEN-QuEChERS methodology were evaluated as extraction and clean up procedures for the simultaneous analysis of 42 organophosphate pesticides in yerba mate (Ilex paraguaiensis). The obtained extracts were analyzed by gas chromatography using a flame photometric detector. Linearity, recovery percentages, relative standard deviations, detection and quantification limits and matrix effects were determined according to DG-SANCO guidelines for both methods. At 0.2 and 0.5mg/kg the evaluated methods showed percentages recoveries between 70 and 120% for most of the analytes. Using Microwave Assisted Extraction methodology, 33 pesticide residues could be properly analyzed whereas only 27 could be determined with the proposed modified QuEChERS. All relative standard deviation were below 18% except for omethoate and disulfoton sulfone when evaluated by the modified QuEChERS. The limits of detection in both methodologies were 0.2mg/kg for most of the analyzed compounds. The average detection limit for QuEChERS was 0.04mg/kg. For 19 of the analytes determined through Microwave Assisted Extraction the lowest validated level were 0.004mg/kg. Signal suppression/enhancement was observed for most of the pesticides, thus matrix-matched calibration curves were used for quantification. The Microwave Assisted Extraction and QuEChERS procedures studied could detect the organophosphate pesticides above the MRL fixed for “mate” by the European Union. They have been successfully applied for the determination of organophosphate pesticide residues in commercial samples and the positives were confirmed through GC–(ITD)-MS.

Highly selective monitoring of metals by using ion-imprinted polymers.

Ion imprinting technology is one of the most promising tools in separation and purification sciences because of its high selectivity, good stability, simplicity and low cost. It has been mainly used for selective removal, preconcentration, sensing and few miscellaneous fields. In this review article, recent methodologies in the synthesis of IIPs have been discussed. For several applications, different parameters of IIP including complexing and leaching agent, pH, relative selectivity coefficient, detection limit and adsorption capacity have been evaluated and an attempt has been made to generalize. Biomedical applications mostly include selective removal of toxic metals from human blood plasma and urine samples. Wastewater treatment involves selective removal of highly toxic metal ions like Hg(II), Pb(II), Cd(II), As(V), etc. Preconcentration covers recovery of economically important metal ions such as gold, silver, platinum and palladium. It also includes selective preconcentration of lanthanides and actinides. In sensing, various IIP-based sensors have been fabricated for detection of toxic metal ions. This review article includes almost all metal ions based on the ion-imprinted polymer. At the end, the future outlook section presents the discussion on the advancement, corresponding merits and the need of continued research in few specific areas. Graphical Abstract IIPs for the selective monitoring of metals.

LA-ICP-MS analysis of natural rock samples using XRF glass beads

Glass beads that remain after measuring major element compositions using XRF can also be used to measure trace element compositions using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The JA-1 and JB-3 reference glass beads were used to evaluate the homogeneity of trace elements contained within them as well as the data quality of LA-ICP-MS measurements. JA-1 has a homogenous trace element composition with less than 10% relative standard deviation, and JB-3 has an average relative standard deviation and average limit of detection of the trace elements of 4% and 0.94%, respectively. The measured and reference values of JB-3 have the highest correlation (R2 = 0.996). Natural rock samples with intermediate to acidic compositions, such as Hwasun andesite, Mudeungsan dacite tuff, and Dogok rhyolite from Mudeungsan National Park, South Korea, are also used to evaluate the LA-ICP- MS data quality. Trace elements in these natural rock samples are plotted in a reasonable area of the geochemical discrimination diagram with sufficient precision. Accordingly, glass beads made from natural rock samples can be used to measure their trace element compositions using fast in situ and low-cost LA-ICP-MS analysis with similar data quality as achieved with normal solution ICP-MS analysis.

Preparation of a new Cu(II)-imprinted polymer and its application for the determination of trace copper in water samples by flame atomic absorption spectrometry

A new Cu(II)-imprinted polymer has been prepared for selective solid-phase extraction of Cu(II) prior to its determination by flame atomic absorption spectrometry. Two functional monomers, 4-(methacryloylamino)benzamide and 4-vinylpyridine, formed a complex with Cu(II) ion through coordination interactions. The self-assembled Cu(II)-monomer complex was copolymerised via bulk polymerisation method in the presence of ethyleneglycoldimethacrylate cross-linker. In order to remove Cu(II) ions, the resulting polymer was washed with 1.0 M HNO3 and then with water until obtaining a neutral pH. The ion imprinted polymer was characterised by Fourier transform infrared. The experimental conditions were optimised for solid-phase extraction of Cu(II) using a column of ion-imprinted polymer (IIP). Quantitative retention was achieved between pH 5.0 and 7.0, whereas the maximum recovery for the non-imprinted polymer (NIP) was about 74% at pH 7.0. The IIP showed higher selectivity to Cu(II) in comparison to the NIP. The IIP also exhibited excellent selectivity for Cu(II) in the presence of other metal ions. The relative standard deviation and limit of detection (3s) of the method were 1.6% and 1.8 µg L−1, respectively. The method was verified by analysis of two certified reference materials (CWW-TM-D and SRM 3280) and then applied to the determination of Cu(II) in seawater and lake water samples and haemodialysis concentrates.

Application of molecular imprinted polymer nanoparticles as a selective solid phase extraction for preconcentration and trace determination of 2,4-dichlorophenoxyacetic acid in the human urine and different water samples.

A molecular-imprinted polymer nanoparticles (MIP-NP) for the selective preconcentration of 2,4-dichlorophenoxyacetic acid (2,4-D) is described. It was obtained by precipitation polymerization from methacrylic acid (the functional monomer), ethylene glycol dimethacrylate (the cross-linker), 2,2′-azobisisobutyronitrile (the initiator) and 2,4-D (the template molecule) in acetonitrile solution. The MIP-NPs were characterized by thermogravimetric analysis, and by scanning electron microscopy. Imprinted 2,4-D molecules were removed from the polymeric structure using acetic acid in methanol (15:85 v/v %) as the eluting solvent. The sorption and desorption process occur within 10 min and 15 min, respectively. The maximum sorbent capacity of the molecular imprinted polymer is 89.2 mg g−1. The relative standard deviation and limit of detection for water samples by introduced selective solid phase extraction were 4.2% and 1.25 μg L−1, and these data for urine samples were 4.7% and 1.80 μg L−1, respectively. The method was applied to the determination of 2,4-D in the urine and different water samples.

Authenticity testing of wheat, barley, rye and oats in food and feed market samples by real-time PCR assays

This work reports four TaqMan real-time PCR assays for authenticity testing of wheat, barley, rye and oat species in food and feed. The method uses three specific primer/probe systems targeting DNA fragments from the ITS1 region for the detection of wheat, barley and oats, and a fourth primer/probe system targeting the MIPS gene for rye detection. The real-time PCR systems showed high specificity and sensitivity, achieving relative detection limits ranging from 0.00001 to 0.01% in an experimental flour binary mixture model. The developed technique was further applied at the field level to check the labeling of 270 food and pet food products regarding the presence/absence of wheat, barley, rye and oat cereals. The assay allowed the authentication of foods with different labeling schemes, in which the presence of the targeted cereals was either declared, not declared or declared as possible traces.

Silver ion imprinted polymer nanobeads based on a aza-thioether crown containing a 1,10-phenanthroline subunit for solid phase extraction and for voltammetric and potentiometric silver sensors

A new nano-sized silver(I) ion-imprinted polymer (IIP) was prepared via precipitation copolymerization using ethyleneglycol dimethacrylate, as a cross-linking agent in the presence of Ag+ and an aza-thioether crown containing a 1,10-phenanthroline subunit as a highly selective complexing agent. The imprint silver(I) ion was removed from the polymeric matrix using a 1.0M HNO3 solution. The resulting powder material was characterized using IR spectroscopy and scanning electron microscopy. The SEM micrographs showed colloidal nanoparticles of about 52nm and 75nm in diameter and slightly irregular in shape for leached and unleached IIPs, respectively. The optimal pH for quantitative enrichment was 6.0 and maximum sorbent capacity of the prepared IIP for Ag+ was 18.08μmolg−1. The relative standard deviation and limit of detection (LOD=3Sb/m) for flame atomic absorption spectrometric determination of silver(I) ion, after its selective extraction by the prepared IIP nanobeads, were evaluated as 2.42% and 2.2×10−8M, respectively. The new Ag+-IIP was also applied as a suitable sensing element to the preparation of highly selective and sensitive voltammetric and potentiometric sensors for ultra trace detection of silver(I) ion in water samples, with limits of detection of 9.0×10−10 and 1.2×10−9M, respectively.

On-line flow injection solid phase extraction using imprinted polymeric nanobeads for the preconcentration and determination of mercury ions

• Presentation of a new analytical method for mercury separation. • Highly selective separation and fast determination of hazardous mercury ion. • Determination of Hg 2+ ion in water and hair samples with acceptable accuracy and precision. • On-line determination of mercury ion based on Hg-IIP NPs through FIA. This work reports a new analytical method for the preconcentration and determination of Hg 2+ ions based on flow injection technique coupled with a solid phase extraction process. Hg 2+ ion imprinted polymeric (IIP) nanomaterials were prepared by using the bulk polymerization procedure, and then applied as an efficient solid phase extractor for selective separation of Hg 2+ ions. The prepared sorbent was characterized using FT-IR spectroscopy, scanning electron microscopy (SEM), various thermal analysis methods, and Brunauer, Emmett, and Teller adsorption isotherm analysis (BET). According to the results, surface area, pore volume and average pore diameter of the prepared Hg-IIP were found to be 3.05 × 10 2 m 2 g −1 , 1.07 cm 3 g −1 and 15.33 nm, respectively. In the sorption studies, after preconcentration and loading of Hg 2+ ions on the IIP sorbent, its mercury content was eluted by suitable solution and then determined photometrically, by a designed on-line recording process coupled with a flow injection procedure. The influence of the mercury concentration, preconcentration and elution times, nature, volume, and concentration of the eluent, pH, and flow rate of the solution and eluent on the polymer affinity has been investigated. Bound Hg 2+ ions can be eluted with 5 mL of nitric acid 1.0 mol L −1 and then treated with diphenylthiocarbazone, finally quantified photometrically at 485 nm. The relative standard deviation and detection limit (3 σ ) of the method for eight replicates at optimum pH, were evaluated as 4.2% and 0.036 ng mL −1 , respectively. The IIP sorbent show an excellent selectivity for Hg 2+ ion over other metal ions and was successfully applied to the selective extraction and determination of Hg 2+ ion in water and human hair samples.

Extraction and separation of polysaccharides from Laminaria japonica by size-exclusion chromatography.

A large number of studies have suggested that polysaccharides, such as fucoidan and laminarin, in various seaweeds have significant biological properties. A different distribution of molecular weights is a prominent sign of many polysaccharides. Therefore, a simple, fast and reliable high-performance size-exclusion chromatography (HPSEC) method was proposed to separate fucoidan and laminarin from Laminaria japonica. After evaluating the different separation conditions for HPSEC, such as the type of mobile phase and flow rate, an acid extraction method was established and optimized by a systematic investigation of the influencing factors. Under the optimal conditions, 169.2 and 383.8 mg g(-1) of fucoidan and laminarin, respectively, were extracted. This method is suitable for the extraction and separation of polysaccharides with good reproducibility of the retention time, acceptable linearity, small relative standard deviation and low detection limits.