• Journal of Genetic Medicine
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• v.4 no.1
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• pp.45-52
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• 2007

Purpose : A simple, rapid, and highly sensitive analytical method for Gb3 in plasma was developed without labor-ex tensive pre-treatment by electrospray ionization MS/ MS (ESI-MS/MS). Measurement of globotriaosy lceramide (Gb3, ceramide trihex oside) in plasma has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. Methods : Only simple 50-fold dilution of plasma is necessary for the extraction and isolation of Gb3 in plasma. Gb3 in diluted plasma was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Results : Eight isoforms of Gb3 were completely resolved from plasma matrix. C16:0 Gb3 occupied 50% of total Gb3 as a major component in plasma. Linear relationship for Gb3 isoforms w as found in the range of 0.001-1.0 ${\mu}g$/mL. The limit of detection (S/N=3) was 0.001 ${\mu}g$/mL and limit of quantification was 0.01 ${\mu}g$/mL for C16:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9678 to 0.9982. Conclusion : This quantitative method developed could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.1
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• pp.85-88
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• 2015

This study attempted to establish an HPLC analysis method for determination of marker compounds as a part of material standardization for the development of health functional food materials from Perilla frutescens Britton var. acuta Kudo. The quantitative determination method of rosmarinic acid as a marker compound of P. frutescens Britton var. acuta Kudo extract (PFE) was optimized by HPLC analysis using a C18 column ($4.6{\times}150mm$, $5{\mu}m$) with 0.1% acetic acid as the elution gradient and methanol as the mobile phase at a flow rate of 1 mL/min and detection wavelength of 280 nm. The HPLC/UV method was applied successfully to quantification of the marker compound in PFE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9995, and the limit of detection and limit of quantitation were $0.36{\mu}g/mL$ and $1.2{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 3.21% and 1.43%, respectively. Recovery rate test at rosmarinic acid concentrations of 12.5, 25 and $50{\mu}g/mL$ scored between 97.04~98.98% with RSD values from 0.25~1.97%. These results indicate that the established HPLC method is very useful for the determination of marker compound in PFE to develop a health functional material.

• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.413-420
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• 2019

In this study, a sample preparation method and a simultaneous determination method by ultra-high performance liquid chromatography coupled with tandem mass spectrometry for 9 isomers of chlorogenic acid and arbutin in fruits were developed. The samples were extracted using 90% methanol (pH 3.0), with the solutions being shaken and then sonicated for 10 min each. After centrifugation at 4,000 rpm for 10 min, the extraction was concentrated under a vacuum at $40^{\circ}C$ using a vacuum evaporator. The residue was dissolved in 5 mL of 5% methanol and filtered through a $0.45{\mu}m$ membrane before UHPLC-MS/MS analysis. The separations were performed on a C18 column with gradient elution of water (containing 0.1% formic acid) and methanol (containing 0.1% formic acid). The specificity, linearity, limit of detection, limit of quantification, accuracy, and precision of the proposed methods were also evaluated.

• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.454-462
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• 2019

A conventional Korean meal typically includes various roasted, steamed, stir-fried, and braised foods. For this study, we investigated the contents of water soluble vitamins, $B_1$ (thiamin), $B_2$ (riboflavin) and $B_3$ (niacin) in various roasted, steamed, stir-fried, and braised foods. Method validation for analytical data in this study showed a high linearity ($r^2$>0.999), and the limit of detection and quantification were 0.001-0.067 and $0.002-0.203{\mu}g/mL$, respectively. For accuracy and precision, analytical values using standard reference materials were in the certified ranges. Roasted foods contained 0.039-1.057 mg/100 g of thiamin, 0.058-0.686 mg/100 g of riboflavin and 0.021-21.772 mg/100 g of niacin. Steamed foods contained 0.049-1.066 mg/100 g of thiamin, 0.025-0.548 mg/100 g of riboflavin and 0.134-21.509 mg/100 g of niacin. Stir-fried foods contained 0.114-0.388 mg/100 g of thiamin, 0.014-1.258 mg/100 g of riboflavin and 0.015-2.319 mg/100 g of niacin. Braised foods contained 0.112-1.656 mg/100 g of thiamin, 0.024-0.298 mg/100 g of riboflavin and 0.322-2.157 mg/100 g of niacin. The data on water-soluble vitamins in this study can be used for a nutritional database of conventional Korean meals.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.30-39
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• 2019

An analytical method was developed for the determination of sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reaction monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges ($0.001-0.25{\mu}g/mL$) into a blank extract with $r^2$>0.99. For validation, recovery tests were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedaxane determination in agricultural commodities.

• Korean Journal of Heritage: History & Science
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• v.38
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• pp.387-419
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• 2005

Material characteristics and provenance interpretation of the raw materials for the stone moulds of bronze artifacts excavated in Galdong Prehistoric site were studied. The stone moulds are made of igneous hornblendite with coarse-grained holocrystalline textures. The surface color shows greenish grey to dark green with greasy luster. The value of magnetic susceptibility of the moulds ranges from 19.2 to 71.0 (mean ; $39.2{\times}10^{-3}$ SI unit).High value of magnetic susceptibility indicates high contents of magnetite as a ferromagnetic mineral and the wide range of the values are due to heterogeneous distribution of magnetite. These are characteristics of basic igneous rocks. The rock-forming minerals of the moulds mainly consist of amphibole, plagioclase and biotite. Pyroxene, chlorite and opaque minerals are also rarely present. A large quantity of carbon was detected on the dark black crust near the surface of the moulds by quantitative analysis. Geological field survey was carried out to identify a source of the raw materials of the stone moulds around Galdong site. Hornblendite or gabbroic rocks being similar to the moulds forming rock occur at Daeseongri, Sikcheonri and Gyodongri in Jangsoo, and Illdaeri in Namwon about 50 kilometers away from the site in a straight line. They have similarity with the moulds forming rock in magnetic susceptibility ranging from 16.1 to 72.4 (mean ; $39.9{\times}10^{-3}$ SI unit). Among those hornblendite or gabbroic rocks, one in Jangsoo area is the most similar to the moulds forming rock on the basis of petrological and mineralogical characteristics. Comparing normalized patterns of major, minor, rare earth and immobile elements contents of the moulds to them of hornblendite in Jangsoo area, geochemical evolution trend and behavior characteristics show affinities between them. It suggests that the moulds forming rock and hornblendite in Jangsoo area have been originated from cogenetic magma. This hornblendite is easy to engrave an inscription or detail graphics on the surface because of its softness, and has good thermal conductivity. Hornblendite in Sikcheonri, Jangsoo is particularly produced and used for stone wares until the present day. Therefore, it is probable that the stone materials of the moulds has been imported from Daeseongri, Sikcheonri and Gyodongri in Jangsoo area. However, it cannot be completely excluded the possibility that the material of the moulds was supplied from Illdaeri in Namwon area appearing the same type of hornblendite on a small outcrops. It is necessary to carry out further archaeological studies to identify several possibilities of migration process of raw materials.

• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.228-238
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• 2021

The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. The extracts were cleaned up using MgSO₄, primary secondary amine (PSA) and octadecyl (C₁₈). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R²) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

• Journal of Practical Agriculture & Fisheries Research
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• v.6 no.1
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• pp.102-115
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• 2004

Main objectives of this study were to increase digestibilities of indigestible ingredients in spent mushroom composts (SMC) consisted of sawdust mainly as well as to fortify conversion of inorganic Se present in SMC to organic Se via fermentable microbial actions. Experimental feeds were designed to contain the increasing level of selenium (0.06ppm, 0.54ppm, 1.26ppm and 1.86ppm) in combination with SMCs of Se-enriched and non-Se mushrooms. Feeds were also fermented using commercial microbial feed additives (Sambae, Ltd., Korea) comprised Saccharomyces, Bacillus, Aspergillus, Streptococcus and Actinomycetes before feeding trial for Hanwoo (Korean native cattle). Those were fermented for 0, 12, 24, and 48 hrs. Initial pH was linearly increased as Se concentration increases or the proportion of SMC of Se-enriched mushroom increased (p<0.0001). pH values of fermented feeds (0.54ppm, 1.26ppm and 1.86ppm) containing SMC of Se-enriched mushroom were not different since 12 hrs of fermentation time and their pH was significantly lowered compared to control group. The increasing level of Se concentration in fermented feeds showed significant differences in organic and inorganic Se contents and proportion of organic Se among treatments. As a SMC proportion of Se-enriched mushrooms in the fermented feed was increased, organic Se proportion was significantly decreased (p<0.0001). The control treatment (0.06ppm) comprising the non-Se SMC only was estimated of the organic Se to be 100% and the treatment groups containing the increasing level of Se were estimated of organic Se to be approximately 70%.

• Analytical Science and Technology
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• v.36 no.6
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• pp.291-299
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• 2023

The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R²) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

• Journal of Food Hygiene and Safety
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• v.39 no.2
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• pp.61-71
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• 2024

In this study, we analyzed chlorogenic acid indicator components in preparation for the additional listing of green coffee bean extract in the Health Functional Food Code and optimized caffeine for simultaneous analysis. We extracted chlorogenic acid and caffeine using 30% methanol, phosphoric acid solution, and acetonitrile-containing phosphoric acid and analyzed them at 330 and 280 nm, respectively, using liquid chromatography. Our analysis validation results yielded a correlation coefficient (R²) revealing a significance level of at least 0.999 within the linear quantitative range. The chlorogenic acid and caffeine detection and quantification limits were 0.5 and 0.2 ㎍/mL and 1.4, and 0.4 ㎍/mL, respectively. We confirmed that the precision and accuracy results were suitable using the AOAC validation guidelines. Finally, we developed a simultaneous chlorogenic acid and caffeine analysis approach. In addition, we confirmed that our analysis approach could simultaneously quantify chlorogenic acid and caffeine by examining the applicability of each formulation through prototypes and distribution products. In conclusion, the results of this study demonstrated that the standardized analysis would expectably increase chlorogenic acidcontaining health functional food quality control reliability.