• Analytical Science and Technology
• /
• v.20 no.3
• /
• pp.251-254
• /
• 2007

In this study, a convenient, fast and accurate inductively coupled plasma atomic emission spectrometry (ICP-AES) method has been optimized for the determination of osmium in aqueous solutions. The method makes use of the reaction of sulfurous acid with osmium to quantitative conversion of volatile Os(VIII) to non-volatile Os(IV) in the pH range 2-10. The response was found to be stabilized immediately after sulfurous acid reacted with osmium. The precision was calculated to be 0.5-4.5 % (RSD) under various ICP-AES conditions. The detection limit was 2.5-57.7 ng/g based on $3{\sigma}$ of the blank response (n=3) using a concentric flow nebulization.

• Journal of Food Hygiene and Safety
• /
• v.34 no.1
• /
• pp.22-29
• /
• 2019

Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

• Journal of the Korean Chemical Society
• /
• v.33 no.2
• /
• pp.208-214
• /
• 1989

A method for the simultaneous determination of copper and cobalt by spectrophotometry has been described. The procedure involves the co-extraction of Cu(Ⅱ) and Co(Ⅱ) from 0.3M HCl into methyl isobutyl ketone as the ion-pairs formed between their thiocyanate complexes and high molecular alkylamines such as Amberlite LA1, Alamine 336, and Aliquat 336. The extract shows the color development to have the maximum absorbances at two different wavelengths i.e., 480 nm for copper and 625 nm for cobalt. Since the spectra of the ion-pairs overlap each other, two simultaneous equations are used to obtain the concentrations from absorbances. Even small amount of Fe(Ⅲ) and Ni(Ⅱ) interferes with the determination of copper. The results of the analysis of samples are in good agreement with the results determined by separate methods within RSD 5.9%.

• Bulletin of the Korean Chemical Society
• /
• v.33 no.9
• /
• pp.3055-3060
• /
• 2012

A simple, rapid and sensitive spectrofluorometric method was developed for the determination of folic acid (FA), based on its quenching effect on the fluorescence intensity of enoxacin (ENX)-europium ($Eu^{3+}$) complex as a fluorescent probe. Fluorometric interaction between ENX-$Eu^{3+}$ complex and FA was studied using UV-visible and fluorescence spectroscopy. The quenched fluorescence intensity at an emission wavelength of 614 nm was proportional to the concentration of FA. Optimum conditions for the determination of FA were investigated. Under optimal conditions, the reduced fluorescence intensity at 614 nm was responded linearly with the concentration of FA. The linearity was maintained in the range of $1.25{\times}10^{-9}$ to $1.50{\times}10^{-7}$ M (R = 0.9986) with the limit of detection ($3S_b/m$) (where $S_b$ is the standard deviation of blank and m is the slop of linear calibration curve) of $6.94{\times}10^{-10}$ M. The relative standard deviation (RSD) for 9 repeated measurements of $1.0{\times}10^{-9}$ M FA was 1.42%. This method was simple, cost effective, and relatively free of interference from coexisting substances. Successful determinations of FA in pharmaceutical formulation and biological samples with the developed method were demonstrated.

• Bulletin of the Korean Chemical Society
• /
• v.34 no.6
• /
• pp.1698-1702
• /
• 2013

Glucose is a common medical analyte measuring in human serum or blood samples. The development of a primary method is necessary for the establishment of traceability in measurements. We have developed an isotope dilution liquid chromatography tandem mass spectrometry as a primary method for the measurement of glucose in human serum. Glucose and glucose-$^{13}C_6$ in sample were ionized in ESI negative mode and monitored at mass transfers of m/z 179/89 and 185/92 in MRM, respectively. Glucose was separated on $NH_2P$-50 2D column, and the mobile phase was 20 mM $NH_4OAc$ in 30% acetonitrile/70% water. Verification of this method was performed by the comparison with NIST SRMs. Our results agreed well with the SRM values. We have developed two levels of glucose serum certified reference material using this method and distributed them to the clinical laboratories in Korea as samples for proficiency testings. The expended uncertainty was about 1.2% on 95% confidence level. In proficiency testings, the results obtained from the clinical laboratories showed about 3.6% and 3.9% RSD to the certified values. Primary method can provide the traceability to the field laboratories through proficiency testings or certified reference materials.

• Journal of Korean Society of Water and Wastewater
• /
• v.18 no.5
• /
• pp.638-648
• /
• 2004

In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of haloacetic acid (HAAs). In this study, headspace solid-phase microextraction (HS-SPME) was studied as a possible alternative to liquid-liquid extraction for the analysis of HAAs in drinking water. The method involves direct derivatization of the acids to their methyl esters without methyl tert-butyl ether (MTBE) extraction, followed by HS-SPME with a $2cm-50/30{\mu}m$ divinylbenzene/carboxen/polydimethylsiloxane fiber. The effects of experimental parameters such as selection of SPME fiber, the volume of sulphuric acid and methanol, derivatization temperature and time, the addition of salts, extraction temperature and time, and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The $2cm-50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, sulphuric acid of 1ml, methanol of 3ml, derivatization temperature of $50^{\circ}C$ derivatization time of 2hrs, sodium chloride salt of 10g, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were selected as the optimal experimental conditions for the analysis of HAAs. The linearities ($r^2$), relative standard deviations (%RSD) and limits of detection (LOD) for HAAs were 0.9978~0.9991, 1.1~9.8% and $0.05{\sim}0.2{\mu}g/l$, respectively.

• Analytical Science and Technology
• /
• v.29 no.1
• /
• pp.29-34
• /
• 2016

This study explores the means by which MX can be effectively extracted from chlorinated water 3-Chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX), a potent mutagen commonly found in chlorinated drinking water at concentrations of up to a few hundred ng/L, was quantitatively determined using sample enrichment followed by liquid-liquid extraction (LLE), derivatization to methylated form, and analysis with GC-MS. A 4-L water sample was enriched to a concentration of 0.4 L using a vacuum rotary evaporator at 30 ℃. MX in the water was extracted using ethyl acetate (100 mL × 2) as a solvent and MX in the extract was methylated with 10 % H₂SO₄ in methanol. MX was recovered at a rate of 73.8 %, which was higher than that (38.1 %) for the resin adsorption method. The limit of quantification and repeatability (as relative standard deviation) were estimated to be 10 ng/L and 2.2 %, respectively. This result suggested that LLE can be used for the determination of MX in chlorinated water as an alternative to more time-consuming resin adsorption method.

• Analytical Science and Technology
• /
• v.33 no.3
• /
• pp.125-133
• /
• 2020

Methylisothiazolinone (MIT) and chloromethylisothiazolinone (CMIT) cause allergic contact dermatitis and are banned cosmetics ingredients, except in rinse-off products. However, their presence has been detected in cosmetics. We report a UPLC-tandem MS/MS screening method for their simultaneous determination in cosmetics. To facilitate extraction from various matrices, pretreatment methods were developed for each sample type. The method was optimized through a series of assessments, including specificity, LOD, LOQ, linearity, recovery, stability, precision, and accuracy. The LODs and LOQs for MIT ranged from 0.054 and 0.163 ㎍ mL^-1 whereas those for CMIT ranged from 0.040 and 0.119 ㎍ mL^-1. The linear correlation coefficients (r²) were higher than 0.999. Relative standard deviations (RSDs) for both intra- and inter-day measurements ranged from 0.3 ~ 13.6 %. Recoveries at three different concentrations were within 87.9 ~ 118.9 %. The RSD for stability measurements of spiked samples was within 7 %. These results confirm the suitability of the developed method for the simultaneous quantitation of MIT and CMIT in cosmetics. Samples of 320 color cosmetics, including eyeshadows, solid lipsticks, liquid lipsticks, and nail polishes were analyzed using the developed method, and two of them were found to contain both MIT and CMIT and one of them was found to contain only MIT. This data and the method will aid the regulation of ingredients used in cosmetics.

• Fisheries and Aquatic Sciences
• /
• v.23 no.3
• /
• pp.9.1-9.6
• /
• 2020

Background: Fucosterol is a compound commonly found in algae that has various biological activities. The purpose of this study was to develop a high-performance liquid chromatography (HPLC) validation method for fucosterol and to compare the fucosterol contents of 11 algal species from Ulleungdo, Korea. Method: In this study, we successfully isolated and identified fucosterol from a 70% EtOH extract of Sargassum miyabei, and subsequently conducted specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision analyses for development of an HPLC validation method. Fucosterol contents were compared using the established HPLC validation conditions. Results: We successfully isolated fucosterol from a 70% EtOH extract of S. miyabei and identified it based on spectroscopic analysis. On the basis of HPLC validation using the fucosterol isolated from S. miyabei, we confirmed specificity (8.5 min), linearity (R² = 0.9998), LOD (3.20 ㎍ mL^-1), LOQ (9.77 ㎍ mL^-1), accuracy (intra-day and inter-day variation, 90-110%), and precision (RSD, 1.07%). Fucosterol contents in the 11 assessed algal species ranged from 0.22 to 81.67 mg g^-1, with the highest content being recorded in a 70% EtOH extract of Desmarestia tabacoides (81.67 mg g^-1), followed by that of Agarum clathratum (78.70 mg g^-1). Conclusions: The results indicate that 70% EtOH extracts of D. tabacoides and A. clathratum containing fucosterol with various effects can be potential alternative sources of fucosterol.

• Korean Journal of Medicinal Crop Science
• /
• v.24 no.4
• /
• pp.271-276
• /
• 2016

Background: In the present study, we established an HPLC (high performance liquid chromatography)-analysis method for the determination of marker compounds as a part of the material standardization for the development of health-functional foods from Salvia plebeia R. Br. extract. Methods and Results: The quantitative determination method of hispidulin as a marker compound was optimized by HPLC analysis using a YMC hydrosphere C18 column with a gradient elution system. This method was validated using specificity, linearity, accuracy, and precision tests. It showed a high linearity in the calibration curve with a coefficient of correlation ($r^2$) of 0.999995. The method was fully validated, and was sensitive, with the limit of detection (LOD) at $0.09{\mu}g{\cdot}m{\ell}^{-1}$ and limit of quantification (LOQ) at $0.27{\mu}g{\cdot}m{\ell}^{-1}$. The relative standard deviation (RSD) values of the data from intra- and inter-day precision were 0.05 - 0.22% and 0.32 - 0.42%, respectively, and the intra- and inter-day accuracy of hispidulin were 99.5 - 102.3% and 98.8 - 101.5%, respectively. The average content of hispidulin in Salvia plebeia R. Br. extract was $3.945mg{\cdot}g^{-1}$ (0.39%). Conclusions: These results suggest that the developed HPLC method is very efficient, and that it could contribute to the quality control of Salvia plebeia R. Br. extracts as a functional ingredient in health functional foods.