Coupled Plasma Mass Spectrometry Method Research Articles

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.

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.

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.

A simple, rapid method for simultaneous determination of multiple elements in serum by using an ICP-MS equipped with collision cell

We developed an inductively coupled plasma mass spectrometry method for testing 23 elements, namely, Mg, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Mo, Cd, Sn, Sb, Ba, W, Tl, Pb, and U, in human serum. The serum samples were analyzed after diluting 1/25 with 0.5% nitric acid, 0.02% Triton-X-100, and 2% methanol. Sc, In, Y, Tb, and Bi were assigned internal standards to correct the baseline drift and matrix interference. The kinetic energy discrimination mode of the instrument with helium gas as the collision gas eliminated polyatomic interference. All 23 elements exhibited excellent linearity in their testing range, with a coefficient of determination ≥ 0.9996. The limits of detection of the 23 elements were within the range of 0.0004–0.2232 µg/L. The intra- and inter-day precision (relative standard deviation) were < 12.19%. The recoveries of the spiked standard for all elements were 88.98–109.86%. Among the 23 elements of the serum reference materials, the measured results of Mg, Al, Cr, Mn, Fe, Co, Ni, Cu, Zn, and Se were within the specified range of the certificate, and the results of the other elements were also satisfactory. The developed method was simple, rapid, and effective, and only 60 μL sample was consumed. A total of 1000 serum samples from healthy individuals were randomly selected from the Henan Rural Cohort, which reflects the status of serum elements in rural adults from the Northern Henan province of central China.

Analytical validation of an inductively coupled plasma mass spectrometry method for urinary iodine concentration measurements in Taiwan

Urinary iodine concentration (UIC) measured by Sandell-Kolthoff spectrophotometric method has been used in the Nutrition and Health Surveys in Taiwan but this method is time consuming and produces toxic waste from arsenic trioxide. The aim of this study was to develop and validate an inductively coupled plasma mass spectrometry (ICP-MS) system to determine UIC in Taiwan. Samples and iodine calibrators were diluted 100-fold into an aqueous solution containing Triton X-100, 0.5% ammonia solution, and tellurium (128Te) as an internal standard. Digestion prior to analysis was not necessary. Precision, accuracy, serial dilution, and recovery tests were performed. A total of 1243 urine samples covering a wide range of iodine concentrations were measured by both Sandell-Kolthoff method and ICP-MS. Passing-Bablok regression and Bland-Altman plots were used to compare values across methods. The limit for detection and quantification by ICP-MS was 0.95μg/L and 2.85μg/L, respectively. The intra-assay and inter-assay coefficients were <10%, with a recovery range of 95%-105%. The results obtained by ICP-MS and the Sandell-Kolthoff method were highly correlated (Pearson's correlation: r=0.996, 95% confidence interval [CI]: 0.9950-0.9961, p<0.001). For UIC between 20 and 1000μg/L, the y-intercept for the Passing-Bablok regression was -1.9 (95% CI: -2.5599 to -1.3500) and the slope was 1.01 (95% CI: 1.0000-1.0206). This validated ICP-MS system can be used for measuring UIC.

Abstract P3-08-03: Establishment of patient-derived xenograft tumor models from breast cancer patients for quantitative elemental profiles and testing candidate therapies

Abstract Breast cancer (BC) is a heterogeneous disease comprising different clinical, histopathological, and molecular subtypes. Triple negative breast cancer (TNBC) is among the most aggressive clinical manifestations of breast cancer (BC), and represents a significant clinical challenge to the effective treatment of early metastatic and treatment-refractory disease because of its poor outcomes. Therefore, there exists a need to develop pre-clinical models that retain the characteristics of the original TNBC tumor—e.g., PDX tumor models—to better understand the mechanisms of drug resistance in metastatic TNBC and to effectively evaluate the effects of anti-cancer drugs on patients with this disease. Furthermore, quantitative changes in cellular element signatures, which indicate levels of enzymatic activity, are emerging new biomarkers for cancer in the clinic, but are of yet systematically understudied in tumor samples from breast cancer patients or/and PDX models of these tumors. Due to limitations in current cellular element signature quantitation profiles, there also exists a need to investigate further. Seven samples of advanced BC patient pleural effusion were obtained from Northwestern Memorial Hospital to establish a PDX tumor model in immunodeficient NSG female mice using breast fat pad xenografting and to develop derived 3D spheroid cultures for anti-cancer drug evaluation. To authenticate, STR profiling against with original patient tumor DNA was conducted. Five developed BC PDX tumor models were shown by pathology to have highly heterogeneous characteristics and the metastatic features of the origin patient tumor. Liver and lung metastases were observed in breast fat pad xenografted PDX tumor mice. 3D tumor spheroid cultures were successfully established from original BC pleural effusion or/and PDX tumor cultures. Using the newly developed, highly sensitive, and reliable Wash-Free Inductively Coupled Plasma Mass Spectrometry (WF ICP-MS) method, we evaluated the inorganic phenotypes from samples of breast cancer patient tumor tissue and of the established PDX tumor to quantify the mobile elements (Na, K, and Ca) and less mobile elements (P, Mg, Mn, Fe, Cu, and Zn) simultaneously within the same sample. The data was collected for further analysis of breast cancer inorganic signatures from normal and tumor cells. Our results suggested that BC 3D spheroid cultures and PDX tumor models could serve as models to further study the mechanisms of MBC and serve as promising tools for in vivo and in vitro quick testing and mechanistic studies of novel antitumor drugs respectively. Identifying quantitative elemental profiles is fundamental to understanding the pathologies of various metal-related cancers and thus opens up new opportunities for disease management and therapeutic intervention Citation Format: Wenan Qiang, Haimei Chen, Yi Yang, Andrew Crawford, Demirkan B. Gursel, Jian-Jun Wei, Thomas O’Halloran, Massimo Cristofanilli. Establishment of patient-derived xenograft tumor models from breast cancer patients for quantitative elemental profiles and testing candidate therapies [abstract]. In: Proceedings of the 2022 San Antonio Breast Cancer Symposium; 2022 Dec 6-10; San Antonio, TX. Philadelphia (PA): AACR; Cancer Res 2023;83(5 Suppl):Abstract nr P3-08-03.

Evaluation of the applicability of the inductively coupled plasma mass spectrometry method for special individual dosimetry monitoring

In the condition of modern radiation hazardous production , higher levels of personnel internal exposure are mainly due to the intake of radionuclides in situations caused by faulty equipment or wrong actions of personnel which can or do result in the exposure that exceeds established standards . In such cases , to determine the intake and committed effective dose , daily amount of urine and / or feces is collected followed by the preparation of loads and their subsequent measurements . For a total , it takes three to eight days to obtain the result depending on the method of measurement used . In case of acute intake of plutonium , it is important to estimate the levels of the nuclide intake as soon as possible in order to decide on treatment strategy and dose reduction . To achieve the above goal , the Southern Urals Biophysics Institute has developed a technique for measuring the plutonium-239 activity in blood using an inductively coupled plasma mass spectrometer as in the first hours and 24 hours after intake ( through inhalation or damaged skin ) the radionuclide concentration in blood is at its maximum level . Also a method has been developed to measure plutonium in urine aliquot using mass-spectrometry to perform special individual dosimetry monitoring that requires almost no sample preparation which allows to estimate the intake within a few hours . It is shown that , depending on the route of intake and chemical form of plutonium compounds entered , the measurement of plutonium activity in blood and urine aliquot performed by the inductively coupled plasma mass spectrometer method allows to determine from 0.1 to 47% of intake limit within the first 24 hours after an accident . The analysis of a blood sample takes one to one - and -a- half workdays against a week required to analyze a urine sample using alpha-spectrometry . The application of the developed methodology , apart from the goal of individual dosimetry monitoring , will provide new information on the effects of chelation therapy on the plutonium behavior in the human body .

Potential human health risks associated with ingestion of heavy metals through fish consumption in the Gulf of Guinea

Heavy metal pollution of the marine environment has toxic implications for both the aquatic biota and human health. We examined the levels of Zinc (Zn), Lead (Pb), Copper (Cu), Cadmium (Cd), Arsenic (As) and Mercury (Hg) in muscles of Sardinella maderensis, Dentex angolensis, Sphyraena sphyraena and Penaeus notialis caught from the coastal waters of Ghana using inductively coupled plasma mass spectrometry method. Penaeus notialis recorded the highest concentrations of all the metals (Cu:12.08±1.46µg/g, Zn: 19.20±2.27µg/g, As: 8.46±2.42µg/g, and Cd: 0.03±0.01µg/g) except Hg. Mercury was relatively high in D. angolensis (0.14±0.03µg/g). Apart from As, all metals were within globally permissible daily limits for consumption by human per meal. The estimated Target Hazard Quotient due to the intake of Hg through D. angolensis consumption exceeded the threshold value across all age categories. Carcinogenic risks due to As intake through P. notialis consumption far exceeded the 10-6 threshold for all age groups in Ghana. It is recommended that the consumption of these fish species particularly, the shrimp P. notialis be done cautiously to avoid possible future health challenges.

Geographical origin traceability of medicine food homology species based on an extract-and-shoot inductively coupled plasma mass spectrometry method and chemometrics

In this work, an extract-and-shoot sample preparation method based on inductively coupled plasma mass spectrometry (ICP-MS) was proposed for fast and efficient geographical origin traceability of medicine food homology species (MFHs). It was not essential to know the absolute contents of mineral elements in MFHs. Exploratory analysis of the MFHs samples was executed by the principal component analysis (PCA) and hierarchical cluster analysis (HCA). The mass spectrometry relative intensities of 46 mineral elements in combination with partial least squares discriminant analysis (PLS-DA) to classify-three MFHs, which were Atractylodis macrocephalae Rhizoma (AMR), Lilii Bulbus (LB), and adlay (AD). Overall, the supervised PLS-DA achieved satisfactory classification results. In addition, variable importance in projection (VIP) was employed to select the main classification indicators. In brief, the proposed method was simple, rapid, environmental, and reliable because it does not require standard solutions of mineral elements and complicated pretreatment, is less time-consuming, and acquires satisfactory results.

Development and Validation of an ICP-MS Method for the Detection of Platinum in the Lebanese Aquatic Environment

Lebanon is a Middle Eastern country located on the eastern Mediterranean coast. Compared to other countries in the MENA (Middle East North Africa) region, Lebanon is considered the richest in water resources. However, due to inadequate water management, Lebanese water resources are under stress. Water pollution is one of the main problems causing major concerns. The contamination of Lebanese surface water originates predominantly from the discharge of untreated municipal and industrial wastewater. With only a few studies investigating the level of water contamination in Lebanon, this research is the first to report the level of platinum in numerous rivers, three wastewater treatment plants, and two untreated sewage outfalls in coastal areas across Lebanon. To determine the platinum levels, an Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) method was developed and validated in compliance with the ICH guidelines. The method demonstrated acceptable sensitivity with LOQ and LOD equal to 2.35 and 0.56 ng L−1, respectively. The level of total platinum in the Lebanese water samples ranged between 22.44–53.32 ng L−1. These concentrations were all above the baseline concentration of platinum in tap water indicated by WHO and aligned with previous studies in other countries. Although the baseline concentration of platinum in Lebanese water resources is unknown and the source of the total platinum detected in this study could not be identified, these preliminary findings could serve as a foundation for future research.

Determination of Mercury with a Miniature Sensor for Point‐of‐care Testing

AbstractIn developing countries, subsistence gold mining entails mixing metallic mercury with crushed sediments to extract gold. In this approach, the gold−mercury amalgam is heated to evaporate mercury and obtain gold. Thus, the highly volatile mercury can be absorbed through inhalation, resulting in adverse health effects. Urinalysis can be used to detect mercury, which is excreted in urine and feces, and correlate exposure with toxic effects. The current gold standard analytical methods are based on fluorescence or inductively coupled plasma mass spectrometry methods, but are expensive, time consuming, and are not easily accessible in countries where testing is needed. In this work, we report on a miniature electrochemical sensor that can rapidly detect mercury in urine at levels well below the US Biological Exposure Index (BEI) limit of 50 ppb (μg/L). The sensor is based on a thin‐film gold electrode and anodic stripping voltammetry electroanalytical approach. The sensor successfully detected mercury at trace levels in urine, with a limit of detection of ∼15 ppb Hg in the linear range of 20–80 ppb. With the low‐cost disposable sensors and portable instrumentation, it is well suited for point‐of‐care applications.

An inductively coupled plasma mass spectrometry method for the determination of elemental impurities in calcium carbonate mineral medicine

Calcium carbonate mineral medicine contains many unknown elemental impurities; however, the detection strategies of the elemental impurities in calcium carbonate differ in various national pharmacopoeias, hindering accurate quantification and risk assessment. In this study, a simple and rapid inductively coupled plasma mass spectrometry method was developed for the detection of 31 elemental impurities in the calcium carbonate mineral medicine by using the collision-reaction cell technique, which could eliminate the mass spectral interference by the complex polyatomic ion. In addition, the isotope ratios were used as a control parameter parameter. The detection result of the proposed method could meet the United States Pharmacopoeia 223, while the risk assessment was performed following the International Conference on Harmonization (ICH) Q3D guidelines. Our results provided a promising strategy for screening and quantitative detection of 31 elemental impurities in calcium carbonate formulations.

Elemental Analysis of Solid Food Materials Using a Reliable Laser Ablation Inductively Coupled Plasma Mass Spectrometry Method.

Quantification of trace and minor nutrient elements is crucial for maintaining human health. A reliable laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method for food materials was developed by combining fine food powder (dm < 3 μm) pellets as the external standard with an average C content as the internal standard (IS). The finer and homogeneous aerosol produced by ablating the fine powder pellets is beneficial for transportation and analyte ionization in ICP, which helps alleviate the matrix effects and improves the analytical precision and accuracy. The average C content is 39.9 ± 1.9% for plant-derived foods (n = 22) and 46.9 ± 1.1% for animal-derived foods (n = 7). The accuracy (recovery, 80-120%) and precision (RSD, 0.5-9.8%) were validated by analyzing a series of food certified reference materials. The high-throughput method is a promising alternative for routine sample analysis in food safety laboratories.

Metal analysis in rice flour

The principal goal of present work was to develop a precise method of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method to measure trace toxic elements (Cd and Pb) and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) method to measure macro and micro elements (K and Cu respectively) in rice flour, the sample preparation method using a system for microwave-assisted pressure digestion and the preparation of laboratory plasticware. The parameters of the sample preparation method, of the spectrometers and measurement results are given.

Determination of Total Arsenic, Soluble Arsenic, Total Mercury and Soluble Mercury for a Realgar and Cinnabar-containing Traditional Chinese Medicine Compound Niuhuang Xiaoyan Capsule by Semi-bionic Extraction- ICP-MS

Background:: Compound Niuhuang Xiaoyan capsule is a realgar and cinnabar-containing traditional Chinese medicine, the contents of total arsenic and total mercury are found over regulation defined limits. However, only a small amount of arsenic in realgar and mercury in cinnabar are dissolved in the gastric juice, so the determination of soluble arsenic and soluble mercury is more significant than that of total arsenic and total mercury in Compound Niuhuang Xiaoyan capsule. Objective: : To study the contents of total arsenic, total mercury, soluble arsenic and soluble mercury in Compound Niuhuang Xiaoyan capsule. Method:: Microwave digestion and semi-bionic extraction were used to pretreat the samples of Compound Niuhuang Xiaoyan capsule, and the inductively coupled plasma mass spectrometry method was established to determine the contents of total arsenic, total mercury, soluble arsenic and soluble mercury in Compound Niuhuang Xiaoyan capsule. The accuracy of the established method was further evaluated by using a certified standard reference material prepared from dried citrus leaves (GBW10020(GSB-11)). Results: : The spiked recoveries were within 95-105 %. The R.S.D% of repeatability (N=6) and precision (N = 6) were below 5.0 %. The correlation coefficients of linear (R) for arsenic and mercury were both above 0.998. The limits of quantification (LOQ) were below 0.1 μg/L. The contents of As and Hg were defined in the dried citrus leaves and very near to the standard values provided by the manufacturer. The established method was applied to the analysis of three batches of Compound Niuhuang Xiaoyan capsule produced by three different manufacturers successfully. Insufficient realgar or cinnabar was formulated in some Compound Niuhuang Xiaoyan capsule samples. Conclusion: : The analysis showed that the contents of soluble arsenic and soluble mercury in artificial gastric juice were significantly less than that of total arsenic and total mercury in Compound Niuhuang Xiaoyan capsule. The results provided a reference for further study on the toxicology and pharmacokinetics of Compound Niuhuang Xiaoyan capsule.