Methotrexate (MTX) is used as an immunosuppressant and antineoplastic drug in clinical practice. MTX is a parent drug and converts to MTX polyglutamates (MTXPGs) to exhibit its biological activity. Clinical studies found that MTXPG levels were associated with MTX response and toxicities, especially at low doses. Due to huge variance of MTX response and toxicities between individuals, therapeutic drug monitoring is necessary for its use in individualized therapy. Various chromatography methods coupled with ultraviolet-visible detector, fluorescence detector and mass spectrometry have been reported for MTXPG analysis in various biological matrices. The aim of this paper is to review the chromatographic based methods for the measurement of total and/or individual MTXPGs. We searched Embase, Science Direct and PubMed databases using “methotrexate polyglutamate” and “chromatography” as search terms, and found 745 articles. Of those, 14 articles were extracted for this study. The key steps for method development (sample pretreatment, parameter optimization of liquid chromatography and mass spectrometry, selection of internal standard) and validation (lower limit of quantitation, accuracy, precision, recovery, matrix effect and stability) were analyzed and summarized, which might be helpful for researchers to develop their own methods.
The identification of cannabis chemotypes at an early stage of a plant’s growth, which is long before anthesis, has been intensively pursued in order to control the on-target selection of the cultivar type at the beginning of cultivation, so as to avoid economic and legal drawbacks. However, this issue has been systematically addressed by only few and relatively recent studies of analytical chemistry, possibly because result validations require long-term monitoring of the content and ratio of cannabinoids and terpenes in a great number of plant specimens suitably selected and grown. Here, we review the procedures, the chromatographic techniques and the statistics used in topical investigations during the past thirteen years. Through heterogeneous and not easily comparable approaches, they prove the feasibility of chemotypes safe determination within the first month of a plant’s life.
A simple visual strategy was developed for the RNase H colorimetric measurement using DNAzyme-mediated signal amplification. When RNase H was presented, the RNA strand of the duplex formed by the G-rich DNA sequence (G-Rich) and its complementary RNA sequence (cp-RNA) was digested, releasing G-Rich to form HRP-mimicking DNAzymes of the G-quadruplex/hemin complexes in the presence of hemin. These DNAzymes catalyze the oxidation reaction of the substrate of 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) to produce green-color products of ABTS•−, allowing for the detection of RNase H. A horseradish peroxidase (HRP)-mimicking DNAzyme of the G-quadruplex/hemin complex was used to mediate the signal amplification in the sensing strategy, resulting in high selectivity and sensitivity. This proposed colorimetric method shows a low detection limit of 0.04 U/mL, with a detection range of 0.1 to 3 U/mL. Moreover, this colorimetric method has been successfully used for RNase H assays in complicated biosamples, such as cell lysates. These results indicate that our colorimetric method not only detects RNase H in an ideal system, but also in real samples.
A simple and novel method for the determination of acetamiprid in water samples is suggested. The method is based on the reducing effect of acetamiprid on the chemiluminescence intensity of new sulfur and nitrogen co-doped carbon dots (S, N-CQDs) in an acetonitrile–hydrogen peroxide (CH3CN–H2O2) system. The possible mechanism was investigated, and it was found that S, N-CQDs react with (1O2)2*, produced from the CH3CN–H2O2 reaction, leading to excited state S, N-CQDs, which deactivate to the ground state by photon emission. Acetamiprid diminishes the chemiluminescence (CL) intensity by competing with S, N-CQDs. The CL intensity reduction is proportional to the concentration of acetamiprid. S, N-CQDs were easily prepared by a hydrothermal method. Under the optimal conditions, a linear range of 2.5 – 25.0 μg L−1 with a detection limit (3σ) of 0.4 μg L−1 was obtained. This method was successfully applied to the determination of trace amounts of residual pesticides in water samples.
It is significant to develop a method for the simultaneous determination of multiple polypeptide antibiotics residues in lake water because of the emergence of multidrug-resistant microorganisms in water. A sensitive, eco-friendly and simple method was developed for the determination of multiple polypeptide antibiotics, including vancomycin, teicoplanin, polymyxin B, colistin and bacitracin A in lake water using liquid chromatography–tandem mass spectrometry (LC-MS/MS). Water samples were lyophilized to enrich them after adjusting the pH to 3. Then, 80% methanol in water containing 0.1% formic acid was used to reconstitute the residues for LC-MS/MS analysis. The results showed that target compounds were well separated and detected under the optimum instrumental conditions. The limits of detection and the limits of quantification of polypeptide antibiotics were in the range of 0.01 – 0.1 and 0.02 – 0.2 ng mL−1, respectively. The matrix-matched calibration curves of all compounds were linear in the calibration range of 1 – 200 ng mL−1. At three spiked levels of 0.2 (0.04), 0.4 (0.1) and 1.0 (0.2) ng mL−1 in lake water, the average recoveries of analytes were higher than 70%, except for teicoplanin, with relative standard deviations of less than 20%. Compared with other common sample pretreatment methods, the lyophilization process is simpler and more eco-friendly, achieving the simultaneous detection of multiple polypeptide antibiotics in lake water. The developed method is successfully applied to the routine monitoring of polypeptide antibiotics residues in lake water.
Alpha-fetoprotein (AFP) is an important disease biomarker, relating to cancers such as hepatocarcinomas and gastric cancer. However, traditional methods are time-consuming, relied on bulky instruments and trained professionals, cannot satisfy the demand for low cost and point-of-care testing (POCT). In this study, a power-free POCT device was developed for the rapid and low-cost detection of AFP via one-sampling. Based on the principle of sandwich immunofluorescence, the chip is capable of automatically accomplishing on-chip mixing, labeling and capturing procedures, which only require that operator add 40 μL sample into the chip one time. The proposed device is capable of sensitively detecting human AFP in FBS with a dynamic range of 10 – 1000 ng/mL and LOD (1.88 ng/mL) within a short time of 3 min. Predictably, our method holds a great potential to be applied in the POC diagnostics of proteins, especially for some regions that are resource-limited.
As a gram-positive foodborne pathogen, Listeria monocytogenes (LM) can cause many serious diseases to the human health coupled with high mortality rates; thus, constructing an effective method to detect LM is of great significance. Herein, a novel sandwich-type electrochemical immunosensor is proposed for LM by introducing 3,4,9,10-perylene tetracarboxylic acid/graphene ribbons (PTCA/GNR) nanohybrids as a sensing platform and ferrocene/gold nanoparticles (Fc/Au NPs) as a signal amplifier. The high conductivity and large surface area of GNR can increase the immobilizing amount of the primary antibody (PAb) and enhance the electron transport rate, while Au NPs can carry secondary antibodies (SAb) and Fc derivative (Fc-SH) to form a SAb-Au NPs-Fc signal amplifier. Through using Fc molecules as a signal probe, its peak current can appear and increase varied from the LM concentrations; hence, a highly sensitive sandwich-type immunosensor was constructed wide linear range from 10 to 2 × 104-CFU mL−1 and low limit of detection of low to 6 CFU mL−1. Furthermore, the specificity of the immunosensor was also studied and a satisfactory result was obtained.
The ion-transfer reactions of alkyl and perfluoroalkyl carboxylate ions (CH3(CH2)n–2COO− and CF3(CF2)n–2COO−) at 1,2-dichloroethane (DCE) | water (W) and 1,1,1,2,3,4,4,5,5,5-decafluoropentane (DFP) | W interfaces were investigated. These ions gave reversible or quasi-reversible voltammetric waves due to their ion transfer across the interfaces, and the formal potentials and the formal Gibbs transfer energies from a non-aqueous solvent to water, ΔG°′tr,α→W (α = DCE and DFP), were determined. The ΔG°′tr,α→W for CH3(CH2)n–2COO− and CF3(CF2)n–2COO− linearly increased with n, allowing for estimating ΔG°′tr,α→W for methylene groups. The estimated value of ΔG°′tr,DCE→W for the –CH2– group was higher than that of ΔG°′tr,DCE→W for the –CH2– group, whereas the ΔG°′tr,DCE→W for the –CF2– group was lower than that of ΔG°′tr,DCE→W for the –CF2– group, indicating that the –CH2– (or –CF2–) group is more favorably (or unfavorably) solvated in the DCE phase compared to the DFP phase. From the estimated values, the fluorination effect of alkyl chains on partitioning the alkyl group between the biphase media has also been discussed.
As a standard method for measuring the concentration of carbonyl compounds in air, 2,4-dinitrophenylhydrazine (DNPH) derivatization followed by high-performance liquid chromatography (HPLC) is widely used. However, the method is often plagued by interference issues related to the ozone content in ambient air samples. Although the use of a potassium iodide (KI) scrubber circumvents these problems, the combination of a DNPH-coated silica cartridge and KI scrubber often performs poorly, particularly in high humidity. The KI in the scrubber becomes wet under these conditions, trapping the carbonyl compounds under investigation before they can reach the DNPH cartridge; this ultimately results in inaccurate readings. In this study, a new type of ozone scrubber consisting of a glass fiber filter coated with hydroquinone (HQF) was developed. The HQF scrubber was placed in front of the DNPH-coated silica cartridge, allowing airborne carbonyl compounds to pass unimpeded through the HQF section before being trapped by the DNPH-coated silica. The subsequent reaction of the trapped carbonyls with DNPH produced carbonyl 2,4-DNPhydrazone derivative that is used as the basis for the quantitative and qualitative analyses of ambient air samples. The hydroquinone in HQF reacts with ozone to form benzoquinone with an efficiency of more than 95% under wide relative humidity range (8 – 95%). The performance of our novel HQF scrubber was compared with those of potassium iodide (KI) and our previously developed trans-1,2-bis(2-pyridyl)ethylene (BPE)-coated silica scrubbers using ambient air samples, and the results showed that both HQF–DNPH and BPE–DNPH cartridges detected carbonyl compounds in the same concentration levels. The proposed method is superior to the KI-based and BPE-based technique for ozone removal because the HQF is very small and can be easily attached to any commercially available DNPH cartridge.
A high concentration of dissolved organic matter is intimately related to the chemistry and ecology of water environments linked to peatlands. To understand the variations in the chemical characteristics of peat derived dissolved organic matter, those in drainage water from natural vegetation and an area containing Sitka spruce (Picea sitchensis), surface water (dubh lochans), and stream water associated with a peatland in central Scotland were analyzed after fractionation into two fulvic acids that were desorbed from an XAD-8 column with water (FAs(H2O)) and 0.1 M NaOH (FAs(NaOH)), humic acids, and dissolved non-humic substances. The elemental composition and the carbon composition as estimated by 13C cross polarisation/magic angle spinning nuclear magnetic resonance did not differ significantly between the FAs(H2O) and FAs(NaOH), whilst the FAs(H2O) were differentiated from the FAs(NaOH) by the greater proportion of carboxy groups with a low pKa at approximately 2. The carboxy group content and the distribution of carboxy groups with respect to the pKa of dissolved non-humic substances were similar to those of FAs(H2O), suggesting their importance as a metal carrier in water systems associated with peatland.
Recently, owing to the performance improvement of the headspace (HS)-sampling devices and its consumables, HS vial samples can be analyzed at temperatures up to 300°C. Some studies have attempted to analyze polycyclic aromatic hydrocarbons (PAHs) in atmospheric 2.5 μm particulate matter (PM 2.5) collected on a filter paper by gas chromatography/mass spectrometry (GC/MS) coupled with thermal desorption device. However, no studies have reported the use of an HS-sampling device to quantify PAHs in PM 2.5 filter paper. In this study, we found that the quantification of PAH analysis using HS-GC/MS can be improved by the following steps, so that the accuracy becomes almost the same as that of a solvent-extraction method: 1) replacement of the air in the HS vial with nitrogen, 2) limiting the solvent to toluene, 3) using the hydrolyzed polyimide-covered septum, and 4) optimization of the heating temperature and heating time of the HS vial. As a result, we succeeded in protecting PAHs in an HS vial at a high temperature and in creating an analysis method with a high recovery rate and high repeatability; the limit of quantitation of each PAH in this method was 5.4 pg m−3 in the case of a volume of 10080 m3 of air being collected on the filter paper.
Existing methods can not achieve rapid mass decomposition and multi-element analysis of graphite ore samples. In this study, it is found that molten lithium metaborate can destroy the structure of graphite, causing graphite C to be oxidized and decomposed in an oxygen environment. We have established a method for testing graphite ore samples with lithium metaborate at 950°C with melting–ultrasonic extraction–ICP-AES multi-element (Al, Ca, Fe, K, Mg, Mn, Na, P, Si, and Ti) testing. The verification results of the national first-level reference materials show that the detection limit of this method is low and the accuracy and precision are good. The results of the measured samples show no significant difference between this method and the classical chemical analysis method. This method has the following advantages over the existing ones: simple operation process, faster decomposition and testing, low reagent consumption, reduced possibility of sample contamination, and better results reproducibility.
This research work aims to propose an extraction method using chitosan as the sorbent and gold nanoparticles (AuNPs) as the colorimetric sensor for the development of a simple, cost-effective, rapid, sensitive, and selective detection method for histidine. The colorimetric assay is based on the aggregation of AuNPs in the presence of Hg2+ ions and histidine. The state of AuNPs generally changes from dispersion to aggregation. The change in state is accompanied by a corresponding change in color (from red wine to blue). Therefore, the solid phase extraction (SPE) method using chitosan as the sorbent was used to extract the AuNPs to improve the sensitivity of detection. It was found that the extraction by means of a sensor system using chitosan could increase the detection signal for histidine by 10 times. The calibration curve, which is the plot of absorbance ratio (A650/A528) against the concentration of histidine, shows a linear relation in the concentration range of 100 – 800 nM. The limit of detection (LOD) and limit of quantitation (LOQ) of the method were found to be 99.88 and 107.45 nM, respectively. Good recoveries were also obtained (range: 99.75 – 104.43%) with relative standard deviations (RSDs) below 5.89% in real water samples. Moreover, this method can be used for the selective detection of histidine even in the presence of other amino acids. The proposed method has been successfully used in the determination of histidine in mineral water samples.
Sunset yellow (SY) is a synthetic colorant which can cause allergies, diarrhea and other symptoms in sensitive people. When ingested too much, it can accumulate in the body and cause damage to the kidneys and liver. Therefore, the content of SY in food must be strictly controlled. In order to regulate their use and ensure food quality, simple and cost-effective methods need to be developed to identify them. In this experiment, fluorescent silicon nanoparticles (SiNPs) were prepared by a one-step method, which is simple, mild and less time-consuming. The fluorescent SiNPs prepared had good thermal stability, excellent salt resistance and pH stability. SY effectively quenched the fluorescence of SiNPs by fluorescence resonance energy transfer when added to the system as an interfering substance. The method had a good linear relationship in the range of SY concentration of 0.050 – 14.0 μg mL−1 and the detection limit is 0.023 μg mL−1. The established sensor was applied to the detection of SY in beverages, and the recovery rate was 93.8 – 102.4%. Based on the excellent selectivity and sensitivity of the method, it could provide a convenient way for the detection of SY in food samples.
Inductively coupled plasma mass spectrometry using isotope dilution (ID-ICP-MS) with liquid–liquid extraction was used for determining ultra-trace tellurium (Te) in steels to improve the sensitivity, accuracy, and precision of the analysis. Single quadrupole-type ICP-MS cannot be used to determine the trace amount of Te because of the contribution of mass spectrometric interference by Xe. To overcome this, tandem mass-filter-type ICP-MS (ICP-MS/MS) was used to determine Te. A pretreatment by liquid–liquid extraction was also employed to compensate for the decrease in the signal intensity due to the use of ICP-MS/MS. The relative standard deviations of the resulting abundances, defined by repeated analysis from separated three steel samples, were <1.3%. Furthermore, the determined values of Te in standard reference materials were close to the reference values. Thus, the developed determination method is useful for the analysis of ultra-trace Te in steels.
Glucose sensors for NMR relaxometry and magnetic resonance imaging (MRI) can be used for the direct measurement of glucose in turbid biological specimens. Here, we proposed a magnetic glucose sensor based on superparamagnetic iron oxide (SPIO) nanoparticles conjugated to a mannopyranoside derivative and concanavalin A (ConA). The binding of mannopyranoside groups to ConA produced a nanoparticle cluster that was dissociated by competitive binding of glucose to ConA, resulting in changes in the transverse relaxation time (T2) in a glucose-dependent manner. The sensor gave rise to significant T2 changes in physiological glucose levels of 3 – 8 mM at a nanoparticle concentration of 0.5 nM. Significant T2 responses were observed within 6 min of 5 mM glucose detection. Sensor-based MRI by a benchtop 1 tesla scanner permitted a measurement of multiple samples within 8 min. These results demonstrate that the relaxometric glucose sensor could lead to high throughput direct assay of blood samples by using a compact MRI scanner for point-of-care testing.
Quantifying total phosphorus contents of organisms can elucidate their physiological condition and the nutrient cycles of ecosystems. Simple, brief, and safe persulfate oxidation methods have been used for total P determination, but oxidizing solutions of different compositions and volumes have been used. Two certified reference materials were used to evaluate digestion efficiencies of different solutions for this study. Although the phosphorus recoveries were low (<90%) without NaOH, phosphorus recoveries using the solution with 4% K2S2O8 and 0.15 M NaOH were complete. Results demonstrated that digestion efficiency depends on the K2S2O8 concentration and on the pH condition. Moreover, the phosphorus recoveries were achieved at >4 mL/mg solution/material ratios for both standard materials. Therefore, the author recommends using >4 mL of the 4% K2S2O8 solution with 0.15 M NaOH for sample materials of <1 mg to quantify the total phosphorus of biological samples.
An analytical investigation was carried out to study the dissipation rate of two commonly used pesticides, thiamethoxam (neonicotinoid insecticide) and propamocarb hydrochloride (carbamate fungicide), applied to four vegetable crops: cucumber, zucchini, lettuce and pepper, after open-field application. Samples were harvested according to a scheduled plan followed by QuEChERS extraction, then thiamethoxam residues were analyzed using a GC-ECD method, while propamocarb HCl residues were analyzed using an HPLC-UV method. Validation parameters were attained for both methods and the kinetic profile was studied, which fitted the first-order kinetics where k, t1/2 and t90 were calculated. The proper pre-harvest interval (PHI) was studied for each crop to ensure that the residues levels declined to reach below the maximum residue limit (MRL) where the crop is suitable for consumption. These values were found to be different from labelled values, which proves that the PHIs are greatly affected by changing weather conditions.
The non-Bornian solvation model has been applied to a theoretical consideration of the Gibbs free energy for the transfer of fluorinated anions, non-fluorinated cations, and non-fluorinated anions at the 2H,3H-decafluoropentane (DFP)/water (W) and 1,2-dichloroethane (DCE)/W interfaces. According to our previous experimental results, the fluorinated anions are more stable in DFP than DCE, while the non-fluorinated cations and anions are less stable in DFP. To understand this characteristic feature of DFP, energy decomposition analyses have been performed for the hypothetical transfer of ions at the DFP/DCE interface. In conclusion, the characteristics of DFP as a fluorous solvent should be explained in terms of the higher repulsive interaction of the solvent molecule with ions, particularly with non-fluorinated ions.
We present a resin-packed microchannel that can reduce the radiation exposure risk and secondary radioactive wastes during uranium (U) separation by downscaling the separation using a microchip. Two types of microchips were designed to densely pack the microchannels with resins. The microchannels had almost the same cross-sectional area, but different outer circumferences. A satisfactory separation performance could be obtained by arranging more than ca. 10 resins along the depth and width of the microchannels. A resin-packed microchannel is an effective separation technique for determining the U concentration via inductively coupled plasma mass spectrometry owing to its ability to avoid the contamination of equipment by cesium, and to reduce the matrix effect. The size of the separation site was scaled down to <1/5000 compared to commonly used counterparts. The radiation exposure risk and secondary radioactive wastes can be reduced by 10- and 800-fold, respectively, using a resin-packed microchannel.
The extraordinary prerequisite for the analysis of an anabolic steroid, namely dianabol (DB), has inspired towards the development of a cost-effective and high-performance sensing probe. Thus, a simple and robust electrochemical sensor (c-MWCNTs-Nafion®lGCE) for dianabol (DB), a widely used steroid, was developed using a glassy carbon electrode (GCE) modified with functionalized carboxylated multi-walled carbon nanotubes (c-MWCNT) and Nafion®. At pH 7 – 8, differential pulse–cathodic stripping voltammetry (DP-CSV) displayed two cathodic peaks at –0.85 and –1.35 V that varied linearly over a wide range (9.0 × 10−9 (2.7 μg L−1) – 9.0 × 10−6 (2.7 × 103 μg L−1) mol L−1) and 2.9 × 10−6 (8.7 × 102 μg L−1) – 8.0 × 10−5 (2.4 × 104 μg L−1) mol L−1) of DB concentrations, respectively. The low limits of detection and quantification at peak I (–0.85 V) were 2.7 × 10−9 (8.1 × 10−1 ng mL−1) and 9.0 × 10−9 (2.7 ng mL−1) mol L−1, respectively. The repeatability and reproducibility displayed relative standard deviations lower than 5%. The method was applied for DB analysis in human urine and subsequently compared with the standard HPLC method. Interference of common metabolites in biological fluids samples to DB sensing was insignificant. This method has distinctive advantages e.g. precise, short analytical time, sensitive, economical, reproducible and miniaturized sample preparation for DB analysis in biological samples of human origin.
129Xe NMR spectroscopy of nanomaterials, such as zeolites, can provide valuable information on the nanostructure and physicochemical properties of adsorption. In the present study the pressure and temperature dependences of the 129Xe NMR chemical shift and the signal intensity were investigated in detail with a zeolite ZSM-5. The pressure dependence of the signal intensity at constant temperature was analyzed based on the Langmuir and Dubinin–Radushkevich (D-R) models, from which the thermodynamic parameters and energetic profiles of adsorption were obtained together with information concerning the nanospace size. From this isotherm analysis the coverage, θ, was calculated and used for isotherm analysis of the chemical shift. The θ dependence of the chemical shift was successfully fitted by an exponential function, and the results were discussed in relation to the chemical shift at zero coverage, that at full coverage and the curvature of the exponential function. The chemical shift data reported with the zeolites NaA and KA, where separated signals were observed for the different number of encapsulated Xe atoms in the α cage, were analyzed and discussed collectively.
Therapeutic oligonucleotides have recently been approved in the United States, the EU, and Japan. Hence, the analysis of oligonucleotides is an important topic in drug development. Liquid chromatographic techniques are commonly used for purity verification and the determination of oligonucleotides. In ion-pair reversed-phase separation, several parameters, such as the pore size of the stationary phase, mobile phase additives, and column temperature, were investigated using three types of oligonucleotides (18, 19, and 20 mer). All of the investigated parameters could influence the separation, and they are expected to be useful for optimizing oligonucleotide separation.
This study aims to provide a simple way to identify the possibility of tetrabromobisphenol A (TBBPA) present in polymers without the need for complicated separation with expensive equipment. Since the presence of phenolic hydroxyl groups is known to be identifiable by the reduction of Fe3+ to Fe2+ in a ferric coloring reagent, the possibility of TBBPA being present in a polymer can be screened by a photometric measurement. A mixed solution of iron(III) nitrate and potassium hexacyanide(III) acid was used as a ferric coloring reagent. With this method, the concentration of TBBPA can be estimated from the photometric absorbance corresponding to the depth of the blue color produced by reduction of the ferric reagent in the presence of Fe(NO3)3. The limit of detection (LOD) was determined to be approximately 2 mg/kg using the Student’s t-test (99% confidence), and a reproducibility of approximately 3% was determined by the relative standard deviation (RSD) from measurements of calibration samples (n = 7). Furthermore, TBBPA in actual polymer samples was screened without the need for any complex processing steps. Because this colorimetric method measures TBBPA by detecting phenolic groups, it may overestimate the TBBPA concentration in the presence of other similar phenolic substances. Nonetheless, this simple colorimetric method should help to quickly identify the presence of TBBPA in various polymers.
A simultaneously HPLC detection method for cannabidiolic acid (CBDA), cannabidiol (CBD), cannabinol (CBN), Δ9-tetrahydrocannabinol (THC), tetrahydro-cannabinolic acid (THCA) in 3 kinds of cosmetics matrix containing hemp leaf extract was developed. The extraction and HPLC conditions were optimized, and a methodological verification was also carried out. The results showed that this method had a good linear relationship in the range of 0.25 – 50 μg/mL with LOD values for 5 cannabinoids all between 0.10 – 0.25 μg/g. The recovery rates of 5 cannabinoids in 3 different cosmetics matrixes were between 90.1 – 108.5%, and the RSD values were all below 4.4%. These results indicated that this method had the advantages of simple operation, high sensitivity, and good accuracy. Through the testing of 6 kinds of hemp cosmetics, it was found that such cosmetics had uneven quality. The establishment of this method can lay a methodological foundation for establishing relevant testing method standards.
A cost-effective long-path absorption liquid core waveguide (LCW) device was fabricated from a typical Teflon tube, and using a high refractive index (RI) medium of acid. It was incorporated in a flow injection–gas diffusion system for the sensitive determination of sulfide via methylene blue (MB) chemistry. The gas diffusion unit could prevent some interferences in samples. The limit of detection of 0.13 μmol L−1 was achieved without using a preconcentration procedure. The proposed device was successfully applied for sulfide determination in canal water samples with 88.7 – 103% recovery.
In this study, single synthetic fibers obtained from several textile products were analyzed by a portable total reflection X-ray fluorescence spectrometer. Characteristic elements, which would originate from such materials as catalysts, delustering agents, and dyes used for manufacturing synthetic fibers, were detected from single synthetic fiber samples, and the difference in the types of characteristic elements among the single synthetic fiber samples was observed.
The ion-exchange selectivity of four metal–organic frameworks (denoted as MLaL), formed by alkali metal ions (M+), La3+, and 1,4-phenylenebis(methylidyne)tetrakis(phosphonic acid) (L), was examined. Unusual selectivity for the alkali metal ions was observed, which did not follow the previously proposed mechanism that was explained based on the ion-size similarity in the framework. The changes in the crystal structures after ion-exchange reactions were observed by powder X-ray diffraction analysis. The change in the lattice energy in a mixed-metal framework is likely to be one of the significant parameters to affect ion-exchange selectivity.
Surface-enhanced laser-induced breakdown spectroscopy (SELIBS) is a promising method for microanalysis of liquid samples. We previously demonstrated that the SELIBS signal was significantly enhanced by using porous silicon (Si) instead of flat Si. In this work, we dried aqueous droplets containing 1 – 200 ppb strontium (Sr) on porous Si substrates and evaluated the quantitative performance by analyzing the dry residues. A linear calibration curve for the Sr quantification (R2 = 0.998) was obtained and an LOD was 0.67 ppb.
In this study, we developed a simple and one-step Pd separation technique based on photoreduction with Xe lamp irradiation for the determination of 107Pd in highly radioactive samples. A simulated high-level radioactive liquid wastes (HLLW) solution, consisting of 14 major elements in a 3 mol L−1 HNO3 solution, was used to evaluate the separation performance. The Pd precipitate was formed by Xe lamp irradiation, and recovered by centrifugation. The Pd recovery from the simulated HLLW solution reached up to 50%, while 99.5% of the other 13 elements was separated. These results indicate that the applicability of the proposed separation technique to HLLW samples.