Plasma Mass Spectrometry Method Research Articles

Co-contamination and interactions of multiple mycotoxins and heavy metals in rice, maize, soybeans, and wheat flour marketed in Shanghai City

Mycotoxins and heavy metals extensively contaminate grains and grain products, posing severe health risks. This work implements validated ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and inductively coupled plasma mass spectrometry (ICP-MS) methods to quantify the concentration of 12 mycotoxins and five heavy metals in rice, maize, soybeans, and wheat flour samples marketed in Shanghai. The mixed contamination characteristics were analyzed using correlation cluster analysis and co-contamination index, and the probabilities of all cross combinations of contaminations were analyzed using a self-designed JAVA language program. The results showed that grains and grain products were frequently contaminated with both mycotoxins and heavy metals, mostly with deoxynivalenol (DON), 3-acetyl-deoxynivalenol (3-ADON), 15-acetyl-deoxynivalenol (15-ADON), ochratoxin A (OTA), aflatoxins, fumonisin B1 (FB1), fumonisin B2 (FB2), fumonisin B3 (FB3), arsenic (As), chromium (Cr) and cadmium (Cd). All the samples (100 %) were contaminated with two or more contaminants, and 77.3 % of the samples were co-contaminated with more than four contaminants. In cereals and cereal products, the following combinations were closely associated: (FB3 +3-ADON), (FB1 +As), (FB1 +FB2), (DON+FB1), (DON+Cd), (As+Cd), (DON+Cd+As), (FB1 +FB2 +As), and (DON+3-ADON+15-ADON). The results indicated that mycotoxins and heavy metals frequently co-occurred in Shanghai grains and grain products, and they provided primary data for safety assessments, early warnings, and regulatory measures on these contaminants to protect public health.

Simultaneous enrichment and speciation of lead and mercury by magnetic solid-phase extraction coupled to HPLC-ICP-MS based on magnetic hydrazine-linked covalent organic frameworks

BackgroundTrace levels of organic and inorganic lead and mercury species in the environment, including divalent lead (Pb2+), trimethyllead (TML), divalent mercury (Hg2+), monomethylmercury (MeHg), and ethylmercury (EtHg), are highly toxic to humans and ecology. It is of great importance for speciation of lead and mercury to evaluate the toxicity of lead and mercury and their biogeochemistry in the environment. However, simultaneous multi-elemental enrichment and speciation at trace level remains a challenge. There are few reports of simultaneous magnetic solid-phase extraction (MSPE) of organic and inorganic lead and mercury species at trace level in the real water. ResultsIn this work, a novel core-shell magnetic hydrazine-linked covalent organic frameworks (Fe3O4@COF-TCH) was prepared for the first time by grafting hydrazine-linked COFs on the Fe3O4 nanoparticles. Fe3O4@COF-TCH with abundant thione and imino groups has strong adsorption for lead and mercury species. Based on it, a simple and practical magnetic solid-phase extraction high-performance liquid chromatography-inductively coupled plasma mass spectrometry (MSPE-HPLC-ICP-MS) method was developed for extraction and determination of trace lead and mercury species, including Hg2+, MeHg, EtHg, Pb2+ and TML. The limits of detection (3δ) of the developed method were 0.08, 0.81, 0.90, 0.56 and 0.88 ng L−1 with the enrichment factors (EFs) of 384, 376, 379, 389 and 360-fold for Pb2+, TML, Hg2+, MeHg and EtHg, respectively. The high accuracy and reproducibility have been proved by the spiked recoveries (94.4–103 %) in real samples. SignificanceThe proposed method with simple operation and high sensitivity has been successfully applied to simultaneous speciation of lead and mercury at trace levels in the water samples with complicated matrices, including underground water, surface water, sea water. Meanwhile, it has the advantages of cost-saving, labor-saving and time-saving and is suitable for the investigation and risk assessment in water. The development of MSPE-HPLC-ICP-MS method provides ideas and guidance for the simultaneous multi-elemental enrichment and speciation.

Pharmacokinetic and Safety Study of Bismuth Potassium Citrate Formulations in Healthy Subjects.

Potassium bismuth citrate is a gastric mucosal protector and a key drug for treating peptic ulcers. To evaluate the pharmacokinetic characteristics and safety of 120-mg bismuth potassium citrate formulations administered orally under fasting conditions in healthy Chinese subjects. A single-center open two-cycle trial was conducted on 12 healthy subjects who received a single oral dose of 120 mg of bismuth potassium citrate. The plasma concentration of bismuth was determined using a validated inductively coupled plasma mass spectrometry (ICP‒MS) method. The pharmacokinetic parameters, including maximum serum concentration (Cmax) and area under the curve concentration-time curve (AUC0-t and AUC0-∞), and safety were evaluated via noncompartment analysis. The ratios of the least square geometric mean ratio between the test (T) and reference (R) formulations for Cmax, AUC0-t, and AUC0-∞ were 44.8%, 55.5%, and 64.4%, respectively; the bilateral 95% confidence intervals (Cis) for these parameters were 20.2-99.6%, 24.1-127.5%, and 23.7-175.0%, respectively, and the non-inferior limits for these parameters were 169.4%, 198.8%, and 200.5%, respectively. The upper limits of the one-sided 97.5% confidence interval for the least squares geometric mean ratio (T/R) were lower than the non-inferior limits. No serious adverse reactions or adverse reactions leading to detachment were observed among the subjects. The concentration of bismuth in the blood of healthy subjects in the T formulation was not greater than that in the R formulation. Similarly, the safety of oral administration of 120 mg of bismuth potassium citrate formulations to healthy subjects was good. The trial registration number (TRN) was [2018] 013, 6 December 2018.

LGYSB:Nd─High-Performance Lasing in the Near-Infrared Region.

Three incongruent melting LawNdxGdyYzSc4-w-x-y-z(BO3)4 (LGYSB:Nd) crystals with different Y concentrations (z = 0.15, 0.05, and 0.025) have been grown by the Czochralski method for the first time. The LGYSB:Nd-type crystals exhibit an acentric structure similar to that of the natural mineral huntite CaMg3(CO3)4, with space group R32. The composition of the LGYSB:Nd_3 (z = 0.025) crystal grown from the starting melt composition La0.628Gd0.547Y0.025Nd0.05Sc2.75(BO3)4 was measured by inductively coupled plasma mass spectrometry method, and it was found to be La0.6794Gd0.4105Y0.0178Nd0.0381Sc2.8542(BO3)4. The transversal spatial distribution of the refractive index in the LGYSB:Nd_3 crystal was investigated. Third-order nonlinear optical susceptibility χ(3) of the LGYSB:Nd_3 crystal was determined from third-harmonic generation experiments with ultrashort (fs) laser pulses. The optical transmission spectrum was measured in the range of 200-2000 nm. The absorption cross-section at 808 nm in σ-polarization was determined to be 1.18 × 10-19 cm2 for the LGYSB:Nd_3 crystal. The 10K absorption spectra revealed that the Nd3+ ions occupy only La3+ cationic sites in the LGYSB host matrix. The emission cross-section at 1064 nm in σ-polarization was determined to be σem(σ) = 1.74 × 10-19 cm2 for the LGYSB:Nd_3 crystal. The fluorescence lifetime was found to be τ = 115 μs for all of the LGYSB:Nd crystals. The LGYSB:Nd_3 laser was operated at an emission wavelength of 1062 nm with very high slope efficiencies of ηsa = 0.74 and ηsa = 0.64 in quasi-cw and cw regimes, respectively.

Ion imprinted polymers integrated into a multi-functional microfluidic paper-based analytical device for trace cadmium detection in water.

A novel multi-functional microfluidic paper-based analytical device (μPAD) integrated with ion imprinted polymers (IIPs) was proposed for specific, portable and low-cost detection of cadmium (Cd(II)) in water. The IIP was grafted on paper and integrated into the μPAD for separation of Cd(II) through multi-layer design. The paper-based screen printed carbon electrode (pSPCE) modified with reduced graphene oxide was fabricated and combined with the μPAD for electrochemical sensing of the separated Cd(II). Reduced graphene oxide (rGO) was prepared via electroreduction on the working electrode surface of the pSPCE (rGO/pSPCE), which provided a sensitization effect with an improved signal for Cd(II) detection. The μPAD developed with the integrated IIP and combined with rGO/pSPCE is able to detect Cd(II) with a linear range from 1 ng ml-1 to 100 ng ml-1 and a detection limit of 0.05 ng ml-1. The accuracy of this μPAD was evaluated with spiked real water samples and compared with that of the inductively coupled plasma mass spectrometry (ICP-MS) method, from which the recovery values ranged from 96.5% to 114.2% with RSDs <10% between the two methods. This μPAD demonstrated its advantages of low-cost, portability, and suitability for highly sensitive detection of Cd(II), making it a valuable tool for on-site analysis.

Performance of single-cell ICP-MS for quantitative biodistribution studies of silver interactions with bacteria

Single-cell inductively couple plasma mass spectrometry (SC-ICP-MS) method development for the study of silver interactions with bacteria to provide information about silver biodistribution in bacteria and spheroplasts.

Determination of trace elements in ibuprofen drug products using microwave-assisted acid digestion and inductively coupled plasma-mass spectrometry

Trace elements are found in most drugs as a result of the drug formulation and drug production methods. An inductively coupled plasma-mass spectrometry method for the determination of 24 trace elements (Mg, Ti, V, Cr, Mn, Cu, Fe, Co, Ni, Zn, As, Se, Mo, Ru, Rh, Pd, Ag, Cd, Sb, Ba, Ir, Pt, Au, and Pb) in solid ibuprofen tablets was established in relation to the ICH Q3D(R1) guideline, to evaluate the possibility of linking trace elemental profiles to drug formulation strategies, and to differentiate between drug products based on the trace elemental profiles. Ten European ibuprofen drug products were evaluated (n=3). The sample preparation was performed by microwave-assisted acid digestion using only 10 mg of homogenized sample and 900 μL of a mix of 65% HNO3, 37% HCl, and 30% H2O2. Solid residuals primarily composed of insoluble SiO2 excipients were removed by centrifugation. Only concentrations of Mg, Fe, Ti, Mn, Cr, and Ni were detected above the limits of detection and did not exceed the ICH Q3D(R1) guideline permitted daily exposure limits. The trace elemental profiles were evaluated through principal component analysis. Three principal components describing 96% of the variance were useful in grouping the ibuprofen drug products, and the detected trace elemental remnants could be related to drug formulation and drug production strategies. An in-house quality control material was used in lack of certified reference materials and was in combination with spike recoveries used for method validation. Good spike recoveries (94–119%) were obtained for all measured trace elements except Mg. Mg showed acceptable spike recoveries (75–155%) for mid and high-spike concentrations, but poor recoveries (30–223%) were detected with low spike concentrations in spike matrices containing high amounts of Mg. Overall, the method is suggested applicable for solid drugs containing insoluble SiO2 excipients and drugs comparable to ibuprofen.

A study on the measurement of GSR with bloodstains by ICP-MS

Abstract In forensic laboratories, analytical investigations of gunshot residues (GSRs) are usually conducted by scanning electron microscopy (SEM) in combination with energy dispersive X-ray (EDX) microanalysis. If GSRs are covered with bloodstains, SEM cannot detect them. In this study, an inductively coupled plasma mass spectrometry (ICP-MS) method is proposed to solve this problem. Results show that bloodstains did not interfere with GSRs and low-level elements are detected. Qualitative and quantitative analyses of Sn, Sb, Ba, and Pb elements in GSRs are also carried out. In addition, testing of GSRs from a type 95–1 rifle and a type 92 pistol is also proposed. Different pretreatment methods are adopted according to the characteristics of different samples. Our investigations suggest that the proposed method has the advantages of low detection limit and high sensitivity and it can be very important in expert testimony.

Matrix-matched calibrators are necessary for robust and high-quality dried blood spots lead screening assays by inductively coupled plasma-mass spectrometry

Background and aimsReliable lead screening methods are necessary to support early identification of lead exposure in children. Sample collection using dried blood spots (DBS) offers advantages compared to traditional venipuncture and capillary collection. Here, we describe and compare three lead DBS inductively coupled plasma-mass spectrometry (ICP-MS) methods for lead screening. Materials and methodsLead was extracted from Whatman 903 protein saver cards punches and analyzed by ICP-MS across three independent clinical laboratories. Each laboratory evaluated the performance of aqueous and matrix-matched DBS calibrators using external quality control samples (WI State of Laboratory of Hygiene Program). Leftover patient samples (n = 39) were used for an interlaboratory comparison of lead DBS. Lead DBS results were compared to whole blood methods. ResultsThe DBS ICP-MS methods using matrix-matched DBS calibrators had superior performance to the aqueous calibrations. There was a strong correlation between lead measured in DBS (matrix-matched) and whole blood for the three methods evaluated. ConclusionLead can be measured accurately by ICP-MS in DBS samples when matrix-matched calibrators are used. External quality control programs are valuable to assess the performance of DBS methods. DBS lead ICP-MS methods are a robust analytical option for lead screening even though the limitations of DBS are well recognized.

Meso–Cenozoic Exhumation in the South Qinling Shan (Central China) Recorded by Detrital Apatite Fission-Track Dating of Modern River Sediments

The Qinling Shan is located between the North China Craton and the South China Block. Not only is investigating the exhumation process of the Qinling Shan beneficial for comprehending the tectonic collision history of mainland China but also for enhancing our understanding of the development of the Yellow and Yangtze Rivers. Previous studies have predominantly focused on bedrock analysis in the Qinling Shan. However, modern fluvial detrital samples offer a more extensive range of thermal history information. Therefore, we gathered modern fluvial debris samples from the Hanjiang River, which is the largest river in the South Qinling Shan. Subsequently, we conducted apatite fission-track analysis using the laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method. A total of 214 valid track ages were obtained, with an age distribution ranging from 9.5 to 334.0 Ma. The Density Plotter software was employed to decompose the data and generate four prominent age peaks: 185, 103, 69, 35, and 12 Ma. The exhumation events of the Early Jurassic (185 Ma) and Cretaceous (103–69 Ma) in the Southern Qinling Shan were strongly influenced by the collision between the South China Block and the North China Craton, as well as the subduction of the West Pacific Plate, respectively. The far-field effect of the collision between the Indian Plate and the southern Asian continent influenced the exhumation of the South Qinling Shan during the Late Eocene (35 Ma) and Middle Miocene (12 Ma), respectively. In conjunction with the reported findings, we comprehensively analyzed the geological implications of the Mesozoic and Cenozoic exhumations of the Qinling Shan. The Qinling Shan emerged as a watershed between the Ordos and Sichuan Basins in the early Mesozoic and Cenozoic, respectively. However, the exhumation and expansion of the Tibetan Plateau has forced the Yangtze River to flow eastward, resulting in its encounter with the South Qinling Shan in the late Cenozoic. The exhumation of the Qinling Shan has resulted in fault depression in the southern Ordos Basin. This geological process has also contributed to the widespread arid climatic conditions in the basin. During the Miocene, the Yellow River experienced limited connectivity due to a combination of structural and climatic factors. As a result, the Qinling Shan served as an obstacle, dividing the connected southern Yangtze River from the northern segment of the Yellow River during the late Cenozoic era.

The geochemistry and geochronology of garnet from the Jinchanghe Fe-Cu-Pb-Zn deposit, Baoshan Block, western Yunnan

The Jinchanghe polymetallic Fe-Cu-Pb-Zn deposit is located in the northern region of the Baoshan Block in western Yunnan. Using electron probe micro-analysis and laser ablation inductively coupled plasma mass spectrometry, we analyzed the major, trace, and rare earth elemental contents of garnets from the Jinchanghe deposit. Moreover, U-Pb dating was performed using the laser ablation sector field inductively coupled plasma mass spectrometry (LA-SF-ICP-MS) method to determine the direct mineralization age of the Jinchanghe deposit. Petrographic analyses revealed three garnet generations: early (GrtI), middle (GrtII), and late (GrtIII). GrtI (And55.69-64.47Gro30.28-41.21Ura + Pyr + Spe + Alm2.35-5.49) was characterized by irregular shapes and weak optical properties, and primarily comprised Fe-rich grossular. GrtII (And53.69-96.17Gro2.78-45.07Ura + Pyr + Spe + Alm0.59-2.12) was characterized by andradite, in which GrtIIa was a homogeneous body, whereas GrtIIb shows exhibited oscillatory zoning with abnormal interference colors. Fine-veined andradite aggregates were predominant in GrtIII (And70.51-90.33Gro6.34-27.80Ura + Pyr + Spe + Alm1.03-3.32). The GrtI, GrtIIa, and the rims of GrtIIb were depleted in heavy rare earth elements and enriched in light rare earth elements, with positive Eu anomalies, indicating that these garnets crystallized from mildly acidic magmatic hydrothermal fluids. However, the cores of GrtIIb had negative Eu anomalies and may have crystallized from a relatively neutral Cl-rich fluid. GrtIII was severely depleted in light rare earth elements with positive Eu anomalies, indicating the presence of a weakly acidic environment. Accordingly, owing to a decrease in temperature and an increase in oxygen fugacity, the pH of the Jinchanghe deposit may have transitioned from an early weakly acidic to neutral, then to a late weakly acidic environment. Furthermore, the ages of GrtII and GrtIII ranged from 520 to 496 Ma, which places the formation of the Jinchanghe deposit during the Late Cambrian. The deposit is closely related to the arc magmatic rocks produced by the subduction of the Proto-Tethys Ocean.

Selenium quantification in wastewaters from selected coal-fired power plants and river waters in South Africa using ICP-MS

South Africa mainly relies on Eskom's coal-fired power plants for electricity generation. However, the use of coal causes several adverse environmental impacts, including the release of selenium into the hydrosphere. Selenium is an essential nutrient for humans, animals, and microbes, but excess selenium is toxic. This paper describes the determination of total dissolved selenium in wastewater from selected coal-fired power plants and river waters near coal-fired power plants in South Africa. A sensitive and robust inductively coupled plasma mass spectrometry (ICP-MS) method for determining total dissolved selenium in wastewater and river water was developed using a certified reference material (NIST SRM 1640a Trace Elements in Natural Water). The results agreed with the certified values, with percentage recoveries ranging from 92–96%. The method detection limit was 0.13 µg/L. Total Se concentrations in wastewater samples from Kriel and Lethabo Power Stations ranged between 4.86 and 8.53 µg/L, and in river water samples from the Olifants and Wilge Rivers, the concentrations ranged from 2.63–8.20 µg/L. These results indicate that the Se levels in the wastewater are too low to pose a health hazard to humans and livestock but pose an environmental threat to aquatic life. The low concentrations in the river samples also show that there may be slight Se pollution (regarding aquatic life) from the selected coal-fired power plants in South Africa. There may be slight Se pollution (with regards to aquatic life) from Duvha and Kendal Power Stations because an increase from 2–8 µg/L was observed in river water samples collected near these selected coal-fired power plants.

Human serum albumin as a copper source for anticancer thiosemicarbazones.

Thiosemicarbazones (TSCs) are a class of biologically active compounds with promising anticancer activity. Their typical mechanism, especially of the clinically far developed representative Triapine, is chelation of iron (Fe), with the Fe-containing enzyme ribonucleotide reductase as primary intracellular target. However, for the subclass of terminally disubstituted, nanomolar-active derivatives like Dp44mT and Me2NNMe2, recent findings suggest that the chelation, stability, and reduction properties of the copper(II) (Cu) complexes are essential for their modes of action. Consequently, it is important to elucidate whether blood serum Cu(II) is a potential metal source for these TSCs. To gain more insights, the interaction of Triapine, Dp44mT or Me2NNMe2 with purified human serum albumin (HSA) as the main pool of labile Cu(II) was investigated by UV-vis and electron paramagnetic resonance measurements. Subsequently, a size-exclusion chromatography inductively coupled plasma mass spectrometry method for the differentiation of Cu species in serum was developed, especially separating the non-labile Cu enzyme ceruloplasmin from HSA. The results indicate that the TSCs specifically chelate copper from the N-terminal Cu-binding site of HSA. Furthermore, the Cu(II)-TSC complexes were shown to form ternary HSA conjugates, most likely via histidine. Noteworthy, Fe-chelation from transferrin was not overserved, even not for Triapine. In summary, the labile Cu pool of HSA is a potential source for Cu-TSC complex formation and, consequently, distinctly influences the anticancer activity and pharmacological behavior of TSCs.

Geobotanical and Biogeochemical Prospecting Method of Complex Sulphide Ore of Pb-Zn-Cu-Ba in Abuni-Adudu areas of the Middle Benue Trough, Nigeria

This research work focused on two plant species namely, the Anogeissus leiocarpus (DC.) and Dichrostachys cinerea for mineral prospecting. The two plants were sampled based on their occurrence, abundance and outlook. Twelve samples (six each of Anogeissus leiocarpus (DC.) and Dichrostachys cinerea) were collected around Abuni-Adudu mining communities in the Middle Benue Trough, Nigeria. In addition, bulk ore and twelve soil samples were also collected and analysed for correlation. Geologically, the study area is made up compacted shale, baked shale (hornfels), and sandstones of sedimentary origin, which are intruded by tertiary basalts of igneous origin. Samples were analysed for elemental composition, using inductively coupled plasma mass spectrometry method. Analysis revealed that the geobotanical method of prospecting for Pb-Zn-Cu-Ba mineralization in the area is promising as biogeochemical data indicated that the Dichrostachys cinerea are good indicator of Pb-Zn-Cu mineralization while the Anogeissus leiocarpus were indicative of Barium. Given the relatively low concentration of Barium in the ore (3.8 ppm) as against concentration in the soil samples, which ranges from 83 ppm (sample YS6) to 552 ppm (sample YS12), Barium has its source from the shale and sandstone or nearby Barite mineralization and not the ore.

Application of mixture analysis methods in association between metals mixture exposure and DNA oxidative damage

Objectives: To study the association between metals mixture exposure and DNA oxidative damage using mixture analysis methods, and to explore the most significant exposure factors that cause DNA oxidative damage. Methods: Workers from steel enterprises were recruited in Shandong Province. Urinary metals were measured by using the inductively coupled plasma mass spectrometry method. The level of urinary 8-hydroxy-2'-deoxyguanosine (8-OHdG) was determined by using the ultra-high performance liquid chromatography-mass spectrometry method. Bayesian kernel machine regression (BKMR), elastic net regression and quantile g-computation regression were used to analyze the association between urinary metals and urinary 8-OHdG. Results: A total of 768 subjects aged (36.15±7.40) years old were included in the study. BKMR, elastic net regression and quantile g-computation all revealed an overall positive association between the mixture concentration and increased urinary 8-OHdG. The quantile g-computation results showed that with a 25% increase in metal mixtures, the urinary 8-OHdG level increased by 77.60%. The elastic net regression showed that with a 25% increase in exposure risk score, the urinary 8-OHdG level increased by 26%. The BKMR summarized the contribution of individual exposures to the response, and selenium, zinc, and nickel were significant contributors to the urinary 8-OHdG elevation. Conclusion: Exposure to mixed metals causes elevated levels of DNA oxidative damage, and selenium, zinc, and nickel are significant exposure factors.

Analysis of Content Profiles, Antioxidant and Anticancer Properties in Endemic Hypericum salsolifolium

This study investigated the antioxidant and anticancer properties, phenolic compounds, and content profile of Hypericum salsolifolium plant extracts prepared with different solvents. The total phenolic content, total flavonoid content, and antioxidant potential [(2,2-diphenyl-1-picrylhydrazyl, 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid), ferric reducing antioxidant power, and cupric reducing antioxidant capacity assays] of Hypericum salsolifolium extracts obtained using solvents of different polarities (hexane, dichloromethane, methanol, and water) were measured using spectrophotometric methods. The contents of the extracts were analyzed using liquid chromatography–mass spectrometry and inductively coupled plasma—mass spectrometry methods. Anticancer detection was performed in human lung carcinoma cells using the 3-4,5-dimethylthiazol-2,5-diphenyltetrazolium bromide, annexin-V, and cell cycle assays, as well as fluorescence detection of acridine orange/ethidium bromide staining. The methanolic extract was determined to have higher activation values of total phenolics, total flavonoids, ferric reducing antioxidant power, and in the 2,2-diphenyl-1-picrylhydrazyl assay than the other extracts, and the aqueous extract had higher values in the 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) and cupric reducing antioxidant capacity assays. The methanolic extract showed a cytotoxic effect against human lung carcinoma cells (IC50: 141.96 µg/mL). It was found that Hypericum salsolifolium extract showed antioxidant and anticancer activities. It was concluded that this plant can be used as a nutritional supplement due to its glucose, phenolic compound, amino acid, and vitamin content.

A Workflow for Uncertainty Assessment in Elemental Analysis of Archaeological Ceramics: A Case Study of Neolithic Coarse Pottery from Eastern Siberia

In this study, the assessment of uncertainties introduced at different stages of the elemental analysis of archaeological ceramics has been described using the example of the Neolithic pottery sherds from Popovsky Lug (eastern Siberia). To evaluate the uncertainty introduced by sampling due to ceramic heterogeneity, three original sherds were cut into small subsamples. Powdered subsamples (250–350 mg) were analyzed using wavelength-dispersive X-ray fluorescence and inductively coupled plasma mass spectrometry methods, and the variations between analytical results for independent subsamples were compared with the variations introduced during the analytical process (measurement and sample preparation). It was shown that 250–350 mg of ceramic is sufficient to obtain good reproducibility (2–15%) between separate subsamples for most major and trace elements, even for the heterogeneous Neolithic ceramics included in this study. The differing behavior of concentration variations in some elements was explained by measuring the ceramic cross-sections by scanning electron microscopy and micro-X-ray fluorescence spectrometry, as well as by the theoretic modeling of the sampling error. The described workflow can be useful in finding uncertainties in elemental analysis results, which may affect the interpretation of bulk chemical composition in ceramic provenance studies.

Determination of cobalt and tungsten in human urine by inductively coupled plasma mass spectrometry

Objective: To establish a inductively coupled plasma mass spectrometry method for the determination of trace cobalt and tungsten in human urine. Methods: The authors used 1% nitric acid solution as diluent in October-December 2021, the sample dilution factor and internal standard element were optimized by single factor rotation experiment, and the difference between the working curve and the standard curve was compared. Results: The method uses working curve to determine cobalt and tungsten in urine, the linear range of this method was 0.0~10.0 μg/L, the correlation coefficient was 0.999 9, the detection limits respectively were 0.005 μg/L (cobalt) and 0.09 μg/L (tungsten), the recoveries of samples respectively were 87.0%~100.2% (cobalt) and 89.4%~104.8% (tungsten), the relative standard deviations respectively were 0.4%~4.4% (cobalt) and 0.6%~3.8% (tungsten) . Conclusion: A simple and rapid method for determination of cobalt and tungsten in urine has been established. This method has the advantages of simple operation, high sensitivity, low detection limit and good stability. It is suitable for determination of cobalt and tungsten in urine of all kinds of people.

Analytical techniques for determination of heavy metal migration from different types of locally made plastic food packaging materials using ICP-MS.

Plastic food packaging is an essential element for customer convenience and the preservation of food quality. Nonetheless, heavy metals in the packaging materials, either intentionally or nonintentionally added, can be transferred to the food. Therefore, determining heavy metal contents in these packaging materials is essential. In this study, heavy metals, including Co, Ge, As, Cd, Sb, Pb, Al, and Zn from different intrinsic plastic food packaging materials were analyzed using the inductively coupled plasma-mass spectrometry (ICP-MS) method. Moreover, the migration of these elements into the environment was also investigated. This method is validated following the new technique's requirements, which include linearity range, accuracy, precision, the limit of detection (LOD), and the limit of quantitation (LOQ). The method has been suitably validated with the regression equation from the standards prepared in HNO3 1% v/v. The linear range was found to be ~1-20 ng mL-1 for Co, Ge, As, Cd, Sb, and Pb and 5-80 ng mL-1 for Al and Zn elements. The LODs are ~0.10, 0.25, 0.12, 0.13, 0.11, 0.12, 0.61, and 0.85 ng mL-1, and the LOQs are 0.33, 0.83, 0.40, 0.43, 0.36, 0.40, 2.01, and 2.81 ng mL-1 obtained for Co, Ge, As, Cd, Sb, Pb, Al, and Zn, respectively. In addition, the recovery percentages received ranged 85.4%-94.1% for Co, 82.6%-95.1% for Ge, 86.3%-97.9% for As, 87.3%-96.3% for Cd, 88.0%-104.4% for Sb, 96.3%-106.0% for Pb, 88.4%-104.0% for Al, and 95.1%-99.7% for Zn. Finally, the migration of these heavy metals from polypropylene (PP) and polystyrene (PS) into foodstuffs was also simulated according to EU legislation, showing that the most leached element was Zn, followed by Al and Pd, with the migration of ~8.38% and ~0.41%, and ~0.19%, respectively.

Establishment of an experimental system for X-ray fluorescence analysis with excitation using 3H/Zr source: Evaluation and applications

The goal of this study is to establish and assess an experimental apparatus for X-ray fluorescence analysis with elemental excitation in materials using a 3H/Zr source. The limits of detection and quantification, as well as analytical sensitivity, were estimated using a linear curve methodology. Furthermore, accuracy and precision were assessed by quantitatively analyzing the components of the reference material. The limits of detection and quantification of elements such as S, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Ta, and Pb were estimated to range from 3.7 mg kg−1 to 573 mg kg−1, depending on the analyte. Analytical sensitivities were found to be between 1.2 and 867 cps/%. The measured elemental concentrations in the reference sample were compared with the inductively coupled plasma mass spectrometry method, and all bias (%) values were found to be lower than 10%. This study also determined the levels of Ca, Ti, Mn, and Fe in cement and K, Ca, Cr, Mn, Fe, and Zn in tea leaves. The results showed that the 3H/Zr source could detect and quantify components at concentrations of a few mg kg−1 or higher. X-ray fluorescence spectrometry is suggested for the analysis of the concentration of various elements in environmental, geological, food, and other samples.