• Korean Journal of Food Science and Technology
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• v.39 no.4
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• pp.372-379
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• 2007

A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.284-289
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• 2017

Oxidized polyethylene wax (OPEW) is, one of the food additives, used as a coating agent in citrus fruits and nuts. OPEW is authorized to quantum satis in EU, USA, and is acceptable less than 250 mg/kg in Australia and New Zealand. But OPEW is unauthorized as a food additive in Korea. This study was to establish the analytical method of OPEW and demonstrate the effective application of various food samples. We first conducted to compare the various analytical method including acid value (AV), high temperature gel permeation chromatography (HT-GPC), matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF/MS), gas chromatography flame ionization detector (GC-FID) and fourier transform infrared spectroscopy (FT-IR). This result indicated that FT-IR spectrum of OPEW treated food sample displayed absorption bands for carbonyl group (C=O, $1714cm^{-1}$), ester group (C-O, $1463cm^{-1}$), aliphatic group (C-H, $2916cm^{-1}$). Furthermore, IR spectrum of OPEW treated food sample showed similar tendency with IR spectrum of OPEW standard. Therefore, it is confirmed that analytical method using FT-IR can be detected on analysis of OPEW in food. As a result of monitoring of 111 samples using established analytical method, OPEW was not detected in the food samples.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.290-297
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• 2017

The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via 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 (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

• Journal of the Korean Geographical Society
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• v.41 no.2 s.113
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• pp.150-167
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• 2006

This study was conducted to determine the pedogenesis of dense subsurface horizons (denoted either Bx or Bd) observed within closed depressions and in toeslope positions at loess-covered glacial tillplains in southern Wisconsin. Some of these dense subsurface horizons, especially those occurring within depressions, show a close morphological resemblance to fragipans elsewhere, even though the existence of fragipans has not been previously reported in southern Wisconsin. The spatial occurrence of fragipans was first examined over the landscape to characterize general soil-landscape relationships. Detailed physico-chemical and micromorphological analyses were followed to investigate the development of fragipans within a closed depression along a catenary sequence. The formation of fragipans at the study site is a result of sequential processes of physical ripening and accumulation of colloidal materials. A very coarse prismatic structure with a closely packed soil matrix was formed via physical ripening processes of loess deposited in small glacial lakes and floodplains that existed soon after the retreat of the last glacier. The physically formed dense horizons became hardened by the accumulation of colloidal materials, notably amorphous Si. The accumulation intensity of amorphous Si varies with mass balance relationships, which are governed by topography and local drainage conditions. Well-developed Bx horizons evolve at closed depressions where net accumulation of amorphous Si occurs, but the collapsed layers remain as Bd horizons at other locations where soluble Si has continuously been removed downslope or downvalley. Hydromorphic processes caused by the presence of fragipans are degrading upper parts of the prisms, resulting in the formation of an eluvial fragic horizon (Ex).

• Journal of the korean academy of Pediatric Dentistry
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• v.31 no.2
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• pp.190-201
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• 2004

The aim of this study was to evaluate the resistance to degradation and to compare the wear resistance characteristics of four esthetic restorative materials in an alkaline solution. The brands studied were Charmfil, Charmfil flow(composite resin), Compoglass F and PrimaFlow(compomer). The results were as follows: 1. The mass loss were not significantly different among the materials(p>0.05). 2. The sequence of the degree of degradation layer depth was in descending order by Compoglass F, PrimaFlow, Charmfil, and Charmfil flow. There were significant differences between Compoglass F and the others(p<0.05). 3. The sequence of the Si loss was in descending order by Charmfil flow, Charmfil, PrimaFlow, and Compoglass F. There were significant differences among these materials(p<0.05). 4. When observed with SEM, destruction of bonding between matrix and filler was observed and when observed with CLSM, the depth of degradation layer of specimen surface was observed. 5. The sequence of maximum wear depth was in descending order by Comfoglass, PrimaFlow Charmal, and Charmfil flow. There were significant differences among these materials(p<0.05). 6. The correlation coefficient between Si loss and degradation layer depth (r=0.602, p<0.05) Vicker's hardness number and maximum wear depth (r=0.501, p<0.05) were relatively high. These results indicate that wear and hydrolytic degradation may be considered to be evaluation factors of composite resins and compomers.

• Journal of the korean academy of Pediatric Dentistry
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• v.32 no.3
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• pp.557-568
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• 2005

The aim of this study was to evaluate the resistance to degradation and to compare the wear resistance characteristics of four esthetic restorative materials in an alkaline solution(0.1N NaOH). The brands studied were MetafilCX(Sun medical, Japan) Solitaire 2(Heraeus Kulzer, USA), Composan LCM(Promedica, Germany), DenFil(Vericom, Korea). The results were as follows: 1. The mass loss of each brand was 0.74~7.94% and highest value in Metafil($7.94{\pm}0.39%$). 2. The sequence of the degree of degradation layer depth was in descending order by Metafil, Solitaire 2, DenFil, Composan LCM. There were significant differences between Metafil and the others(p<0.05). 3. The sequence of the Si loss was in descending order by Metafil, Solitaire 2, Composan LCM, DenFil. There were significant differences among the materials(p<0.05). 4. On SEM, destruction of bonding between matrix and filler and on CLSM, the depth of degradation layer of specimen surface was observed. 5. The sequence of maximum wear depth was in descending order by Metafil, Solitaire 2, Composan LCM and DenFil. There were significant differences among the materials(p<0.05). 6. The correlation coefficient between Si loss and degradation layer depth (r=0.491, p<0.05) and Vicker's hardness number and maximum wear depth (r=-0.942, p<0.05) were relatively high. These results indicate that hydrolytic degradation and wear may consider as a evaluation factors of composite resins.

• 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 Food Hygiene and Safety
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• v.30 no.3
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• pp.272-280
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• 2015

A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.

• Korean Journal of Environmental Agriculture
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• v.37 no.4
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• pp.283-290
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• 2018

BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.

• 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.