• Economic and Environmental Geology
• /
• v.43 no.5
• /
• pp.443-453
• /
• 2010

The Samsung gold-silver deposit consists of quartz veins that fill along the fault zone within Cretaceous shale and sandstone. Mineralization is occurred within fault-breccia zones and can be divided into two stages. Stage I is main ore mineralization and stage II is barren. Stage I is associated with wall-rock alteration minerals(sericite, pyrite, chlorite, quartz), rutile, base-metal sulfides(pyrrhotite, pyrite, sphalerite, chalcopyrite, galena), and electrum. Stage II occur quartz, calcite and pyrite. Fluid inclusion data indicate that homogenization temperatures and salinities of stage I range from 145 to $309^{\circ}C$ and from 0.4 to 12.4 wt.% NaCl, respectively. It suggests that hydrothermal fluids were cooled and diluted with the mixing of meteoric water. The main deposition of base-metal sulfides and electrum occurred as a result of cooling and dilution at temperature between $200^{\circ}C$ and $300^{\circ}C$. Sulfur(9.3~10.8‰) isotope composition indicates that ore sulfur was mainly derived from a magmatic source as well as the host rocks. The calculated oxygen[-2.3~0.9‰(quartz: 0.3‰, 0.9‰, calcite: -2.3‰)] and hydrogen[-86~-76‰(quartz: -86‰, -82‰, calcite: -76‰)] isotope compositions indicate that hydrothermal fluids may be meteoric origin with some degree of mixing of another meteoric water for paragenetic time.

• Analytical Science and Technology
• /
• v.27 no.2
• /
• pp.92-99
• /
• 2014

Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

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

• Analytical Science and Technology
• /
• v.28 no.6
• /
• pp.460-466
• /
• 2015

An isotope dilution liquid chromatography tandem mass spectrometry was developed as a primary method for the quantitative analysis of cholesterol in infant formula. Cholesterol-d₄ was used as an internal standard and spiked into the infant formula sample. In order to release cholesterol out of cholesteryl ester, which is cholesterol bound to fatty acids in infant formula, saponification was carried out. Saponification conditions were optimized with heating temperature, reaction time and the concentration of KOH. The optimum conditions were as follows; heating temperature was 70 ℃, reaction time was 180 min and the concentration of KOH was 0.8 mL of 8 M KOH for about 0.1 g infant formula sample. Extraction of cholesterol out of sample solution was carried out with hexane uisng liquid-liquid extraction. Chromatographic analysis was carried out using Phenomenex Kinetex C₁₈ column. Mobile phase was 0.1% acetic acid in methanol/water (v/v, 99/1) and flow rate was 0.3 mL/min. Cholesterol and cholesterol-d₄ were monitored at mass transfer m/z 369/259 and 373/263 respectively. Reproducibility of the method was evaluated to be 0.23% of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9% at a 95% confidence level. NIST standard reference material having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM within the uncertainty.

• Journal of The Korean Society of Grassland and Forage Science
• /
• v.27 no.3
• /
• pp.167-172
• /
• 2007

Manure recycle is an emerging issue in agriculture in Korea these days. Farmers are keeping eye on legume mixture with grasses for nitrogen fixation and transfer to companion crops by legumes. We had a trial to investigate the effect of different legume mixtures on nitrogen fixation and transfer in spring soil. The treatment was arranged in a randomized complete block design with three replications. Three different mixtures were used(rye+hairy vetch, Italian ryegrass+crimson clover, oat+pea) and sowed in pots with paddy soil from western part of Korea(Seo Chon County). Pots with rye+vetch were transplanted from field of RDA(rural development administration) in Suwon on 2 February 2007 and other mixture treatments were sowed on early March with different sowing rate(7:3=Italian:crimson, 6:4=oat:pea). $(^{15}NH_4)_2SO_4$ solution at. $99.8\;atom%^{15}N$ was applied to the each pot at the rate of $2kg\;N\;ha^{-1}$. Application was done on 6 April at rye+vetch pots and remainder were applied on April 16. Forage were harvested from each pot at ground level in heading stage and separated into legume and grass. Total N content and $^{15}N$ value were determined using a continuous flow stable isotope ratio mass spectrometry. DM yield of rye+vetch, Italian+crimson and oat+pea were 6,607, 3,213 and 4,312 kg/ha, respectively. Proportion of N from fixation was 0.73(rye+vetch), 0.42(Italian+crimson) and 0.93(oat+pea). The percentages of N transfer from legume to grass were from 61% to 24% in different method by treatment and -35% to 21% in isotope dilution method.

• Toxicological Research
• /
• v.31 no.3
• /
• pp.255-264
• /
• 2015

Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, $A{\alpha}C$, $MeA{\alpha}C$, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including $IQ-d_3$, $MeIQx-d_3$, $PhIP-d_3$, $Trp-P-2-^{13}C_2-^{15}N$ and $MeA{\alpha}C-d_3$ was spiked for quantification of HCAs and $^{13}C_3$-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.

• Analytical Science and Technology
• /
• v.26 no.5
• /
• pp.307-314
• /
• 2013

Selenium exists in various forms of chemical species. The activity and bioavailability is strongly dependent on its chemical form and concentration. Consequently the information on each selenium species and its concentration must be exactly determined for the food we take in. In this study, selenium species in seafood were separated and quantified by RP (reversed phase) HPLC (high performance liquid chromatography) coupled with ICP-MS (inductively coupled plasma mass spectrometry) using post-column isotope dilution. $^{79}Br$, which interferes on $^{80}Se$, has mostly been removed by solid phase extraction and then mathematical correction has been applied for the more accurate correction. The experimental result for CRM (certified reference material) DOLT-4 agreed well with the certified value but each selenium species could not be compared. SeCys (selenocysteine) and SeMet (selenomethionine) were the major species detected in seafood such as belt fish, spanish mackerel, and squid that have been serving as Korean diet. The concentrations found in Korean sea food for SeCys and SeMet were in the range of 0-661.6 mg/kg and 137.3-462.7 mg/kg, respectively.

• Journal of the Korean Chemical Society
• /
• v.63 no.5
• /
• pp.335-341
• /
• 2019

Spirulina was cultured in Selenium solution and the total concentration was determined with isotope dilution technique. Low-molecular-weight-Selenium species for the water extract of Spirulina were separated and quantified with HPLC ICP/MS. Water extraction was used first and then protein enzyme (protease XIV) was used to digest and extract for the Se species in both water extract and residue. The total Se was $414.9{\pm}4.0{\mu}g\;g^{-1}$ and 77% existed in water extract while 22% remained in residue. Se species in supernatant was mostly inorganic selenate ($222.7{\mu}g\;g^{-1}$). After hydrolysis of protein, SeCys ($15.20{\mu}g\;g^{-1}$) and SeMet ($12.13{\mu}g\;g^{-1}$) were found. In residue, SeCys and SeMet were found with little inorganic Se. After protein hydrolysis of residue, more of Selenoamino acids SeCys ($9.35{\mu}g\;g^{-1}$) and SeMet ($18.23{\mu}g\;g^{-1}$) in addition to MeSeCys ($1.5{\mu}g\;g^{-1}$) were found. It is thought that inorganic selenium is mostly adsorbed on the surface of spirulina and can be easily removed by a simple distilled water extraction while most of organo-seleniums are remained in residue.

• Analytical Science and Technology
• /
• v.21 no.5
• /
• pp.364-374
• /
• 2008

Antarctic Environmental Monitoring Handbook' was published by COMNAP/SCAR in 2000. The standardized method described in this handbook is recommended for monitoring of antarctic environment. High pressure bomb technique in this guide was used to decompose soil samples. In compliance with this guide book, high pressure bomb technique was applied to decompose the antarctic soil sampled at the King Sejong Station. An Isotope Dilution-Inductively Coupled Plasma-Mass Spectrometry (ID-ICP-MS) was applied to determine mass concentrations of Pb, Cu and Zn in the soil. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of NIST 2702 (marine sediment). The analytical results agreed with certified value within the range from 99.5~100.8%. Matrix separation was necessitated for the determination of Cu and Zn by Chelex 100 ion exchange resin. As a result, the average mass concentrations of Pb, Cu and Zn which are suspected to be caused by anthropogenic pollution were 332.9 mg/kg, 95.6 mg/kg and 115.3 mg/kg, respectively. Those for the metals sampled in the soils of the remote regions from the station were 28.1 mg/kg, 101.8 mg/kg and 115.6 mg/kg, respectively.

• Analytical Science and Technology
• /
• v.37 no.3
• /
• pp.166-173
• /
• 2024

Steroids have a temporary skin improvement and whitening effect by controlling vasodilation, but they also cause side effects when used for a long time. Therefore, steroids were designated and managed as raw materials that cannot be used in cosmetics in Korea. However, steroids are continuously being detected in cosmetics, causing social issues. In this study, we developed a certified reference material (CRM) for the determination of steroids such as hydrocortisone in cosmetics. A cream-type cosmetic CRM was manufactured and subsequently certified following the guidelines outlined in ISO Guide 35. Homogeneity, short-term stability, and long-term stability were evaluated using isotope dilution mass spectrometry (ID-MS). The certified values were determined by using NIST's primary reference material to ensure traceability. From now on, we intend to supply the certified reference material as a cosmetic CRM to national and international companies, as well as research institutes after certification as certified reference material from KOLAS and registering on COMAR.