• Analytical Science and Technology
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• v.28 no.6
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• pp.417-424
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• 2015

In this study, the relationship between selenoprotein concentrations in blood and stomach cancer have been searched for Korean. The concentration of each selenoprotein in blood serum was analyzed and the correlation between the concentration and stomach cancer was studied to find a potential for using Selenium as a biomarker. In concentration determination, a simple calibration curve method was used with the monitoring of m/z 78 without the use of solid phase extraction. This is a lot more simple than the method using SPE with post column isotope dilution. The result obtained from the analysis of CRM BCR-637, 72.20±3.35 ng·g⁻¹, showed similar value of reference value (81±7 ng·g⁻¹). The total concentration of Se for the controlled group, cardiovascular patients group, was 105.70±21.20 ng·g⁻¹. This value was the same as normal healthy person reported earlier. Each selenoprotein concentration of GPx, SelP and SeAlb was 26.12±7.84, 65.15±14.50, 14.43±6.99 ng·g⁻¹, respectively. The distribution of each selenoprotein was 24.7%, 61.6%, and 13.7%, which was similar to the normal person. The result of stomach cancer patients, the total concentration of Se was 76.11±28.12 ng·g⁻¹ and each concentration of GPx, SelP and SeAlb was 15.41±9.01, 50.83±17.91, and 9.87±5.21 ng·g⁻¹, respectively. The total and each selenoprotein concentration level showed significant decrease for the stomach cancer patients. The level of decrease was 41.0% for GPx, 22.0% for SelP, and 31.6% for SeAlb. However, the distribution of each selenoprotein was not much different. Either total Selenium or each selenoprotein could be used as a possible index for the diagnosis of cancer. However, in age group study, it is shown that young age group (30's-40's) did not show much difference.

• Journal of Food Hygiene and Safety
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• v.26 no.1
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• pp.16-24
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• 2011

A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

• Analytical Science and Technology
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• v.24 no.5
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• pp.345-351
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• 2011

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

• Analytical Science and Technology
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• v.28 no.5
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• pp.323-330
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• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

• Tuberculosis and Respiratory Diseases
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• v.42 no.1
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• pp.84-92
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• 1995

Background: Nasal applied continuous positive airway pressure(CPAP) is a highly effective method of treatment for obstructive sleep apnea syndrome. More than a decade of accumulated experience with this treatment modality confirmed that it is unquestionably the medical treatment of choice for patients with obstructive sleep apnea syndrome. However it takes long time to reach optimal CPAP pressure. To save the time to reach optimal pressure, it is necessary to clarify the time to reach optimal pressure for treatment of obstructive sleep apnea syndrome. Method: CPAP pressure is titrated during an overnight study according to a standardized protocol. Just before the presleep bio-calibration procedures, the technician applies the nasal mask and switches on the clinical CPAP unit. Initial positive for pressure is typically 3.0 centimeters of water pressure. After sleep onset, the technician gradually increases the pressure until sleep-disordered breathing events disappear or become minimal. The pressure must maintain maximal airway patency during both NREM and REM sleep to be considered effective. Before recommending a final pressure setting, sleep recording and oximetry data are reviewed by an American Board of Sleep Medicine certified Sleep Specialist and a Registrered Polysomnographic Technologist. Results: We examined the time required to reach optimal pressure during routine CPAP titration in 127 consecutively evaluated individuals diagnosed with sleep-disordered breathing. Results indicate that 33% of patients required more than four hours to attain satisfactory titration. This indicates that a four-hour session is marginally enough time, at best, to determine a proper CPAP pressure setting. Moreover, 60 of 127 patients required further adjustment after optimal pressure was reached. These additional pressure trials were needed to confirm that higher pressures were not superior for eliminating sleep-disordered breathing events. Conclusions: The data presented underscore the logistical difficulty of titrating CPAP during split-night studies without modifying the titration procedure. Futhermore, the time needed to reach optimal pressure makes it improbable that proper CPAP titration can be performed during a 2-3 hour nap study.

• Journal of the Korean Society of Food Science and Nutrition
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• v.43 no.6
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• pp.955-961
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• 2014

This study was carried out to investigate the amounts of vitamin C in 22 sweet potato cultivars cultivated in Korea as well as evaluate the effects of cooking methods on vitamin C contents. Methods for determining vitamin C was validated by determining linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy using HPLC. Results showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9999. The LOD and LOQ values for ascorbic acid (AA) were 0.03 and $0.10{\mu}g/mL$, respectively. The relative standard deviations (RSDs) for intra- and inter-day precision of AA were less than 5%. The recovery rates of AA and dehydroascorbic acid (DHA) were in the range from 98.21~98.64 and 98.28~100.68%, respectively. Depending on cultivar, contents of AA, DHA, and total ascorbic acid (TA) in sweet potatoes varied in the range from 37.76 (Sinyulmi)~89.25 (Juhwangmin), 23.37 (Sinjami)~63.94 (Sinyulmi), and 68.52 (Sinjami)~115.95 (Juhwangmin) mg/100 g, respectively, and their average levels were $56.98{\pm}12.53$, $36.46{\pm}9.03$, and $93.44{\pm}12.00mg/100g$, respectively. The average TA levels were also dependent on flesh color, whish was significantly higher in general sweet potato and orange sweet potato than in purple sweet potato. Steaming, baking, and frying processes significantly reduced AA (10.61~58.41%), DHA (2.57~52.81%), and TA (14.54~49.92%) contents in sweet potatoes. The highest reduction of AA, DHA, and TA contents was observed after baking, followed by steaming and frying. We expect that the basic information provided by this study will be useful to plant breeders and food scientists.

• Analytical Science and Technology
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• v.25 no.3
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• pp.171-177
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• 2012

A determination method of aromatic amino acids such as trytophan (Trp), tyrosine (Tyr), and phenylalanine (Phe) using luminol-$H_2O_2$-Cu(II) system has been presented. In the presence of an aromatic amino acid, the enhanced chemiluminescence (CL) intensity of luminol-$H_2O_2$-Cu(II) system was obtained by forming a complex between Cu(II) and the amino acid. Based on the above phenomenon, a sensitive and fast determination of three aromatic amino acids was performed using the CL method in batch-type detection system. To optimize determination conditions, the kinetic influence of an aromatic amino acid on the luminol-$H_2O_2$-Cu(II) system and the effects of $H_2O_2$ and Cu(II) concentration, pH, and buffers were investigated. Under the optimized conditions, the calibration curve was linear over the range from $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Trp, $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Try, and $2.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Phe, respectively. In this range, reproducibility (RSD, n = 4) of Trp, Try, and Phe were 3.21%, 2.64%, and 2.48%, respectively. The limit of detection ($3{\sigma}/s$) was calculated to be $6.8{\times}10^{-7}\;M$ for Trp, $5.7{\times}10^{-7}\;M$ for Try, and $9.6{\times}10^{-7}\;M$ for Phe.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.329-335
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• 2017

Analysis method was presented for the simultaneous determination of nine bisphenol A related compounds such as bisphenol A (BPA), phenol, p-tert-butylphenol, bisphenol A diglycidyl ether (BADGE), $BADGE{\cdot}2H_2O$, $BADGE{\cdot}2HCl$, bisphenol F diglycidyl ether (BFDGE), $BFDGE{\cdot}2H_2O$ and $BFDGE{\cdot}2HCl$ migrated from inner coatings of metal food cans by high performance liquid chromatography (HPLC) with fluorescence detection. The method was validated by examining the linearity of calibration curve, the limit of detection (LOD), the limit of quantification (LOQ), recovery and uncertainty. The migration tests of nine BPA related compounds were carried out with four food simulants; deionized water (DW), 4% acetic acid, 50% ethanol and n-heptane. There was not any compound detected in DW, 4% acetic acid and 50% ethanol at $60^{\circ}C$ for 30 min and n-heptane at $25^{\circ}C$ for 60 min. BPA and phenol were migrated into 4% acetic acid and 50% ethanol at $95^{\circ}C$ for 30 min. The concentrations were ranged from 0 to $10.77{\mu}g/L$ of BPA and from 0 to $2.35{\mu}g/L$ of phenol. Canned foodstuffs mostly have long-term shelf life. We investigated migration of nine BPA related compounds according to the variation in storage periods (0~90 days) and temperatures (4, 25 and $60^{\circ}C$). All compounds were not founded during 90 days at $4^{\circ}C$ and $25^{\circ}C$, respectively. However BPA and $BADGE{\cdot}2H_2O$ were founded in DW and 4% acetic acid at $60^{\circ}C$. The migration levels of BPA and $BADGE{\cdot}2H_2O$ were close to the value of LOQ, respectively and did not change significantly as storage period. It was founded from results that the migration of BPA related compounds from metal food cans was controlled to a safe level.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.274-281
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• 2015

BACKGROUND: A lasting release of low levels of persistence chemicals including pesticides and pharmaceuticals into river has a bad influence on aquatic ecosystems and humans. The present study monitored pesticide residues in the Yeongsan and Seomjin river basins and their tributaries as a fundamental study for water quality standard of pesticides.METHODS AND RESULTS: Nine pesticides(aldicarb, carbaryl, carbofuran, chlorpyrifos, 2,4-D, MCPA, methomyl, metolachlor, and molinate) were determined from water samples using SPE-Oasis HLB(pH 2) and LC/MS/MS. Validation of the method was conducted through matrix-matched internal calibration curve, method detection limit(MDL), limit of quantification(LOQ), accuracy, precision, and recovery. MDLs of all pesticides satisfied the GV/10 values. Linearity(r²) was 0.9965- 0.9999, and a percentage of accuracy, precision, and recovery was 89.4-113.6%, 3.1-14.0%, and 90.8-106.2%, respectively. All pesticides exclusive of aldicarb were determined in the river samples, and there was a connection between the positive monitoring results and agricultural use of the pesticides.CONCLUSION: Monitoring outcomes of the present study implied that pesticides were a possible non-point pollutant source in the Yeongsan and Seomjin river basins and tributaries. Therefore, it is required to produce and accumulate more monitoring results on pesticides in river waters to set water quality standards, finally to preserve aquatic ecosystems.

• Journal of Food Hygiene and Safety
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• v.33 no.3
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• pp.176-184
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• 2018

The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.