• Analytical Science and Technology
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• v.36 no.5
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• pp.216-223
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• 2023

Aluminium (Al) is one of the major elements in rocks and its concentration can be varied, depending on different rock types as well as sources. The present study aimed to propose an analytical method based on the UV-Vis as a cheap, simple, and common instrument equipped in most laboratories for Al quantification in rocks after the microwave assisted acid digestion. The aluminone and 8-hydroxyquinoline were investigated for the colorimetric assay. The results show that the 8-hydroxyquinoline reagent was more favorable in terms of the minimized affects of the potential interferences present in the digested solutions, i.e., Fe³⁺, Si⁴⁺ and F^-. The calibration curve was constructed from 0.10 mg/L to 3.00 mg/L with the goodness of linearity (R² = 0.9996). The limits of detection and quantification (LOD and LOQ) were estimated, i.e., 0.029 mg/L and 0.087 mg/L, respectively. The 8-hydroxyquinoline was applied to real rock samples, demonstrating favorable precision (RSD = 0.34 %-1.8 %) and no remarkable differences were found compared to the inductively coupled plasma-mass spectrometry (ICP-MS) as a reference measurement approach.

• Journal of Preventive Medicine and Public Health
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• v.56 no.5
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• pp.422-430
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• 2023

Objectives: Prolactin is vital for breastfeeding and milk production, and its secretion is influenced by factors related to the mother, infant, and environment. To date, no study has concurrently investigated the correlation of these factors with serum prolactin levels during lactation. Therefore, the objective of this study was to investigate the correlations among maternal and infant factors, lead exposure, and serum prolactin levels during lactation. Methods: A cross-sectional approach was employed in Surabaya, Indonesia, among 110 exclusively lactating mothers. The mothers' daily diets were determined using multiple 24-hour recalls, while blood lead levels were measured with inductively coupled plasma mass spectrometry. Serum prolactin levels were assessed using the electrochemiluminescence immunoassay. For bivariate analysis, we employed the Spearman correlation, Mann-Whitney, and Kruskal-Wallis tests, while for multivariate analysis, we utilized multiple linear regression. Results: The average serum prolactin level of the lactating mothers was 129.19±88.96 ng/mL. Positive correlations were found between serum prolactin levels and breastfeeding frequency (p<0.001), protein intake (p<0.001), and calcium intake (p=0.011) but had negative correlation with blood lead levels (p<0.001) and vitamin B6 intake (p=0.003). Additionally, prolactin levels were not significantly associated with maternal age; parity; intake of calories, vitamin D, vitamin E, zinc, folic acid, magnesium, or iron; infant age; or infant sex. Conclusions: Breastfeeding frequency had a stronger positive relationship with serum prolactin levels than protein and calcium intake. However, lead exposure was associated with reduced serum prolactin levels during lactation. Consequently, specific interventions from policymakers are necessary to manage breastfeeding in mothers exposed to lead.

• Analytical Science and Technology
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• v.28 no.5
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• pp.309-316
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• 2015

The analytical method of lead in plasma by ICP-MS was validated after securing environment within class 1,000 classification. We tested specificity and accuracy of within-run and between-run. According to measurement of the amount of suspended particulates in a clean room, 0.3~62 particles were detected in 0.3 µm size while 0.0~28.3 particles were observed in 0.5 µm size. Total suspended particulates met required environment with up to 90.3 particles. The MDL (Method detection limit) of the sample which has been fabricated using fetal bovine serum (FBS) blank was 1.77 ng/L, and LOQ (Limit of quantification) was 5.55 ng/L. The slope, intercept and correlation coefficient of the calibration curve were y=1.09×10⁻³x+4.88×10⁻² and r=0.9999, which showed good correlation. The specificity, within-run and between-run accuracy satisfied the standard at more than 50 ng/L. The average lead concentration in plasma of the general people, current workers and retired workers was 55.4 ng/L, 440 ng/L, and 132 ng/L.

• Analytical Science and Technology
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• v.29 no.5
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• pp.234-241
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• 2016

The approach presented in this article refers to the bioanalytical method validation for the detection and quantitative determination of arsenic species including arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) in dog plasma by high-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP/MS). The arsenic species were separated using an agilent As speciation column by a mobile phase of 2 mM sodium phosphate monobasic, 0.2 mM ethylenediaminetetraacetic acid disodium salt dehydrate, 10 mM sodium acetate, 3 mM sodium nitrate and 1 % ethyl alcohol at pH 11 (adjusted with 1M NaOH). The method validation experiment was obtained selectivity, linearity, accuracy, precision, matrix effect, recovery, system suitability, dilution integrity and various stabilities. All calibration curves showed good linearity (R²>0.999) within test ranges. The lower limit of quantitation (LLOQ) was 5 ng/mL for As(III), As(V) and DMA, and 20 ng/mL for MMA. The system suitability and dilution values were within 6.5 % and 7.7 %. Subsequently, the developed and validated HPLC-ICP/MS method was also successfully applied to determine the arsenic speciation in dog plasma samples, and the recoveries for the spiked samples were in the range of 91.5–102.2 %. Therefore, this method could be applied to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies in biological samples.

• Analytical Science and Technology
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• v.15 no.5
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• pp.417-426
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• 2002

Inductively Coupled Plasma Dynamic Reaction Cell Quadrupole Mass Spectrometry (ICP-DRC-QMS) was characterized for the detection of the six naturally occurring calcium isotopes. The effect of the operating conditions of the DRC system was studied to get the best signal-to-noise ratio. This experiment shows that the potentially interfering ions such as $Ar^+$, ${CO_2}^+$, ${NO_2}^+$, $CNO^+$ at the calcium masses m/z 40, 42, 43, 44 and 48 were removed by flowing $NH_3$ gas at the rate of 0.7 mL/min $NH_3$ as reactive cell gas in the DRC with a RPq value (rejection parameter) of 0.6. The limits of detection for $^{40}Ca$, $^{42}Ca$, $^{43}Ca$, $^{44}Ca$, and $^{48}Ca$ were 1, 29, 169, 34, and 15 pg/mL, respectively. This method was applied to the determination of calcium in synthetic food digest samples (CCQM-P13) provided by LGC for international comparison. The isotope dilution method was used for the determination of calcium in the samples. The uncertainty evaluation was performed according to the ISO/GUM and EURACHEM guidelines. The determined mean concentration and its expanded uncertainty of calcium was ($66.4{\pm}1.2$) mg/kg. In order to assess our method, two reference samples, Riverine Water reference sample (NRCC SLRS-3) and Trace Elements in Water reference sample (NIST SRM 1643d), were analyzed.

• The Journal of the Petrological Society of Korea
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• v.20 no.3
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• pp.161-172
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• 2011

Open beaker digestion method is routinely used as the sample preparation technique for trace element determination of rock samples by inductively coupled plasma mass spectrometry, With this method, however, dissolution of Zr and Hf is not always guaranteed especially when the samples contain refractory minerals. In this study, glass bead digestion technique was compared with conventional open beaker digestion technique for the sample preparation of three USGS rock standards such as AGV-2, BHVO-2, and G-3. Thirty trace elements including rare earth elements were analysed by ICP-MS and ICP-AES. There were no clear differences in analytical results for the AGV-2 and BHVO-2 standards between the two techniques, but Zr, Hf, Y, and middle- to heavy- rare earth element concentrations of the G-3 standard prepared by open beaker digestion technique were significantly lower than the recommended values. This can be attributed to the presence of refractory mineral zircon. On the contrary, all the analytical results of the G-3 standard prepared by glass bead digestion technique were in good agreement with the recommended values, indicating complete dissolution of zircon. The analytical results show that the volatile elements such as Pb and Zn were not lost during the preparation of glass bead. Low dilution glass bead digestion technique described here will be very helpful to enhance precision and accuracy of trace element analysis for geological samples containing refractory minerals.

• Journal of Environmental Health Sciences
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• v.49 no.2
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• pp.66-77
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• 2023

Background: Along with the increase in consumer interest in and consumption of tattoo products, the controversy over harmful heavy metals associated with the use of tattoo cosmetics is also increasing. Therefore, investigation of hazardous metals in these tattoo products is needed. Objectives: This study was performed to provide useful data for establishing reasonable standards to securely manage tattoo cosmetics, tattoo stickers, and tattoo inks distributed in the market. Methods: Thirteen kinds of hazardous metal contents (Pb, As, Cd, Sb, Ni, Co, Cu, Cr, Se, Ba, Zn, Sn, and Hg) were analyzed for 23 tattoo cosmetics, ten tattoo stickers, and 16 tattoo inks. Hg was measured through the combustion-gold amalgamation method, and other hazardous metals were measured by inductively coupled plasma-mass spectrometry (ICP-MS) after acidic decomposition using a microwave apparatus. Results: The detected ranges of Pb, As, Cd, Sb, Ni, and Hg in tattoo cosmetics were 0.07~1.18, 0.06~0.41, ND~0.07, 0.01~3.44, 0.12~2.75, and ND~0.01 ㎍/g, respectively. All of the hazardous metals detected were below the recommended maximum standards of the Ministry of Food and Drug Safety. The mean amount of Pb detected in tattoo stickers for children was 0.24 ㎍/kg and Cd was not detected, meaning both metals met the recommended criteria. There was no statistically significant difference in all measured metals between children's tattoo stickers and adults' tattoo stickers. In the results of the study on the hazardous metal content of tattoo inks, four products (25%) for Pb, one product (6%) for As, 13 products (81%) for Ni, four products (25%) for Cu, and five products (31%) for Zn exceeded the recommended standards approved by the government. The highest predicted exposure amount for hazardous metals exceeding the recommended level of tattoo inks in a single tattooing was 5.69 ㎍/kg for Ni, 8.51 ㎍/kg for Zn, 0.44 ㎍/kg for Pb, 8.07 ㎍/kg for Cu, 0.44 ㎍/kg for As, and 71.36 ㎍/kg for Ba. Conclusions: It is necessary to prepare criteria for content limitation for the management of Co, Cr, Ba and Se tattoo cosmetics, and tattoo inks require thorough quality control.

• Analytical Science and Technology
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• v.16 no.5
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• pp.358-367
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• 2003

In this research, first of all, the analytical methods for the determination of major elements in sediment have been developed with ICP-MS (Inductively Coupled Plasma Mass Spectrometry). The analytical results of major elements (Al, Ca, K, Fe, Mg) with Cool ICP-MS were much better than those with normal ICP-MS. The analytical results were compared with those of NAA (Neutron Activation Analysis). NAA were a little superior to ICP-MS for the determination of major elements in sediment as a non-destructive trace analytical method. The analytical methods for the determination of minor elements (Cr, Ce, U, Co, Pb, As, Se) have been also developed with ICP-MS. The analytical results by standard calibration curve with ICP-MS were not accurate due to the matrix interferences. Thus, the internal standard method was applied, then the analytical results for minor elements with ICP-MS were greatly improved. The analytical results obtained by ICP-MS were compared with those obtained by NAA. It showed that the two analytical methods have great capabilities for the determination of minor elements in sediments. Accordingly, the NAA will play an important role in analysis of environment sample with complex matrix. ICP-MS also will play an important role because it has a great capability for the determination of Pb that could not be determined by NAA.

• Journal of Environmental Health Sciences
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• v.41 no.5
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• pp.289-298
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• 2015

Objectives: The method of analyzing urinary arsenic by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) is generally used because it shows relatively greater sensitivity, low detection limits, low blocking action, and is simple to operate. In this study, the results of analysis according to three pre-reductants commonly used in the FI-HG-AAS method were compared with each other. Methods: To analyze urinary arsenic, nineteen urine samples were collected from adults aged 43-79 years old without occupational arsenic exposure. Analysis equipment was FI-HG-AAS (AAnalyst 800/FIAS 400, Perkin- Elmer Inc., USA). The three pre-reductants were potassium iodide (KI/AA), C3H7NO2S (L-cysteine), and a mixture of KI/AA and L-cysteine (KI/AA&L-cysteine). Results: In the results of the analysis, the recovery rate of the method using KI/AA was 82.3%, 95.7% for Lcysteine, and 123.5% for KI/AA and L-cysteine combined. When compared with the results by use of high performance liquid chromatography inductively-coupled plasma mass spectrometry (HPLC-ICP-MS), the method using L-cysteine was the closest to those using HPLC-ICP-MS ($98.57{\mu}g/L$ for HPLC-ICP-MS; $74.96{\mu}g/L$ for L-cysteine; $69.23{\mu}g/L$ for KI/AA and L-cysteine; $13.06{\mu}g/L$ for KI/AA) and were significantly correlated (R2=0.882). In addition, they showed the lowest coefficient of variation in the results between two laboratories that applied the same method. Conclusion: The efficiency of hydride generation is considered highly important to the analysis of urinary arsenic via FI-HG-AAS. This study suggests that using L-cysteine as a pre-reductant may be suitable and the most rational among the FI-Hg-AAS methods using pre-reductants.

• Analytical Science and Technology
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• v.11 no.4
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• pp.271-280
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• 1998

Rice flour reference materials were prepared from the unpolished rice grown in Korea and certified for elemental composition. The reference materials consist of two samples containing normal and high level. The reference material at elevated level was prepared by spiking to the normal rice flour six toxic elements of As, Cd, Cu, Cr, Hg, Pb with $1.0{\mu}g/g$ on a dry weight basis. Homogeneity of the prepared materials was evaluated through the determination of Ca, Cu, Fe, Mn, Zn by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). Small variance of elemental composition among interbottled samples assured homogeneity of the prepared materials. The materials were decomposed by high pressure digestion and microwave digestion method. INAA, AAS, inductively coupled plasma-atomic absorption spectrometry (ICP-AES), ICP-mass spectrometry (MS) and vapour generation techniques were employed to analyze the reference materials. From this independent analytical results, the certified or reference values are determined for As, Ca, Cd, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, P, Pb, Se, Zn.