• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.381-388
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• 2017

In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.

• Korean Journal of Food Science and Technology
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• v.42 no.1
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• pp.8-13
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• 2010

Bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE) were obtained by a polymerization reaction of epichlorohydrin (ECH) with bisphenol A (BPA) or bisphenol F (BPF). These compounds are commonly used as monomers or additives such as a polymerization stabilizer and a hydrochloric acid scavenger of epoxy resin, polyvinyl chloride (PVC)-containing organosols and polyester lacquers, that are applied to the internal surface of most canned foods to impart chemical resistance. The unreacted BADGE, BFDGE and their reaction products migrating from epoxy resin, PVC-containing organosol and/or polyester lacquer-based food packaging materials into the foods have recently become an issue of great concern because of increased customer demand for safety. This study was conducted to develop a rapid and sensitive simultaneous analysis method based on HPLC/FLD and HPLC/APCI-mass and to evaluate the concentration of BADGE, BFDGE and their metabolites, BADGE $H_2O$, BADGE $2H_2O$, BADGE HCl, BADGE 2HCl, BADGE HCl $H_2O$, BFDGE $H_2O$, BFDGE $2H_2O$, BFDGE HCl, BFDGE 2HCl and BFDGE HCl $H_2O$ for 133 canned food samples. The method provided a linearity of 0.9997-0.9999, a limit of detection of $0.01-0.13\;{\mu}g/mL$, a limit of quantitation of $0.03-0.44\;{\mu}g/mL$ and a recovery (%) of 85.64-118.18. The number of samples containing BADGE, BFDGE or their metabolites were: 28/133 (21.1%), with levels of 0.400-0.888 mg/kg being observed for aqueous foods (19/133) and 0.093-0.506 mg/kg being observed for oily foods (9/133).

• 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 the Korean Society of Food Science and Nutrition
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• v.46 no.10
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• pp.1186-1194
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• 2017

Recently, many people have demanded reliable nutritional data even for minor-components. On the other hand, an analytical method for the analyses of vitamin $B_5$ and $B_6$ is lacking. Therefore, this study attempted to validate with accuracy and precision the analysis of vitamin $B_5$ and $B_6$ using a high-performance liquid chromatography (HPLC) method. The vitamin $B_5$ and $B_6$ contents were analyzed using an Agilent 1260 series HPLC system. YMC-Pack ODS-AM ($250{\times}4.6mm$ I.D.) and YMC-Pack Pro RS $C_{18}$ ($250{\times}4.6mm$ I.D.) columns were used for the analyses of vitamin $B_5$ and $B_6$, respectively. In the case of vitamin $B_5$, the flow rate was set to 1.0 mL/min by isocratic elution using the 50 mM $KH_2PO_4$ solution (pH 3.5)/acetonitrile (ACN) (95:5, v/v) with monitoring at 200 nm using HPLC/DAD, whereas the flow rate for vitamin $B_6$ was set to 1.0 mL/min of flow rate by isocratic elution using a 20 mM $CH_3CO_2Na$ solution (pH 3.6)/ACN (97:3, v/v) with monitoring by excitation at 290 nm and emission at 396 nm using HPLC/FLD. The column temperature was set to $30^{\circ}C$. The injection volume was $20{\mu}L$ for each experiment. The specificity of the accuracy and precision for vitamin $B_5$ and $B_6$ were also validated by HPLC. The results showed high linearity in the calibration curve for vitamin $B_5$ ($R^2=0.9998^{{\ast}{\ast}}$), the limit of detection (LOD) and limit of quantitation (LOQ) were 0.4 mg/L and 1.3 mg/L, respectively, In contrast, for the calibration curve of vitamin $B_6$, which showed high linearity ($R^2=0.9999^{{\ast}{\ast}}$), the LOD and LOQ were 0.006 mg/L and 0.02 mg/L, respectively.

• 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 Korean Society of Environmental Engineers
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• v.31 no.2
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• pp.79-89
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• 2009

Naphthalene is a volatile, hydrophobic, and possibly carcinogenic compound that is known to have a severe detrimental effect to aquatic ecosystem. Our research examined the effects of various operating conditions (temperature, pH, initial concentration, and frequency and type of ultrasound) on the sonochemical degradation of naphthalene and OH radical production. The MDL (Method detection limit) determined by LC/FLD (1200 series, Agilient) using C-18 reversed column is measured up to 0.01 ppm. Naphthalene vapor produced from ultrasound irradiation was detected under 0.05 ppm. Comparison of naphthalene sonodegradion efficiency tested under open and closed reactor cover fell within less than 1% of difference. Increasing the reaction temperature from $15^{\circ}C$ to $40^{\circ}C$ resulted in reduction of naphthalene degradation efficiency ($15^{\circ}C$: 95% ${\rightarrow}$ $40^{\circ}C$: 85%), and altering pH from 12 to 3 increased the effect (pH 12: 84% ${\rightarrow}$pH 3: 95.6%). Pseudo first-order constants ($k_1$) of sonodegradation of naphthalene decreased as initial concentration of naphthalene increased (2.5 ppm: $27.3{\times}10^{-3}\;min^{-3}\;{\rightarrow}$ 10 ppm : $19.3{\times}10^{-3}\;min^{-3}$). Degradation efficiency of 2.5 ppm of naphthalene subjected to 28 kHz of ultrasonic irradiation was found to be 1.46 times as much as when exposed under 132 kHz (132 kHz: 56%, 28 kHz: 82.7%). Additionally, its $k_1$ constant was increased by 2.3 times (132 kHz: $2.4{\times}10^{-3}\;min^{-1}$, 28 kHz: $5.0{\times}10^{-3}\;min^{-1}$). $H_2O_2$ concentration measured 10 minutes after the exposure to 132 kHz of ultrasound, when compared with the measurement under frequency of 28 kHz, was 7.2 times as much. The concentration measured after 90 minutes, however, showed the difference of only 10%. (concentration of $H_2O_2$ under 28 kHz being 1.1 times greater than that under 132 kHz.) The $H_2O_2$ concentration resulting from 2.5 ppm naphthalene after 90 minutes of sonication at 24 kHz and 132 kHz were lower by 0.05 and 0.1 ppm, respectively, than the concentration measured from the irradiated M.Q. water (no naphthalene added.) Degradation efficiency of horn type (24 kHz) and bath type (28 kHz) ultrasound was found to be 87% and 82.7%, respectively, and $k_1$ was calculated into $22.8{\times}10^{-3}\;min^{-1}$ and $18.7{\times}10^{-3}\;min^{-1}$ respectively. Using the multi- frequency and mixed type of ultrasound system (28 kHz bath type + 24 kHz horn type) simultaneously resulted in combined efficiency of 88.1%, while $H_2O_2$ concentration increased 3.5 times (28 kHz + 24 kHz: 2.37 ppm, 24 kHz: 0.7 ppm.) Therefore, the multi-frequency and mixed type of ultrasound system procedure might be most effectively used for removing the substances that are easily oxidized by the OH radical.

• Analytical Science and Technology
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• v.26 no.4
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• pp.287-297
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• 2013

The optimization of analytical method for the thermal desorption of seven VOCs (volatile organic compounds) by TD-GC/MS (thermal desorption-gas chromatograph-mass spectrometer) with solid phase sorbent tube, and comparative analysis for the determination of VOCs plotted by standard sorbent tubes prepared using both gas phase and liquid phase materials were investigated. The result of paired t-test showed that a liquid phase standard sorbent tube method was in agreement with a gas phase standard sorbent tube method for six species of VOCs including benzene, toluene, ethylbenzene, o-, m-, and p-xylene except for styrene at the significance level (${\alpha}=0.01$), while the 15.6% of difference in response factor between both of gas phase and liquid phase standard plotting for the determination of styrene showed that both methods were significantly different at the significance level. Therefore, the liquid phase standard plotting method was employed to reduce erroneous data for the determination of styrene including BTEX. Under the optimized analytical method by liquid phase standard sorbent tube, recovery was between $100{\pm}5%$ for 7 species of VOCs, reproducibility ranged from 0.3 to 7.7%, and method detection limit (MDL) ranged from $0.01{\mu}g/m^3$ for o-xylene to $0.27{\mu}g/m^3$ for toluene. The optimized standard method was applied to determine VOCs VOCs from indoor air of of dormitory, one bedroom apartment, and a new car.

• 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.34 no.2
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• pp.148-157
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• 2019

An optimized analytical method for sodium iron chloriphyllin in foods was established and verified by using high performance liquid chromatography with attached diode array detection. An Inertsil ODS-2 column and methanol-water (80:20 containing 1% acetate) as a mobile phase were employed. The limit of detection and quantitation of sodium iron chloriphyllin were 0.1 and 0.3 mg/kg, respectively, and the linearity of calibration curve was excellent ($R^2=0.9999$). The accuracy and precision were 93.9~104.95% and 2.0~7.7% in both inter-day and intra-day tests. Recoveries for candy and salad dressing were ranged between 93 and 104% (relative standard deviation, (RSD) 0.3~4.3%), and between 83 and 115% (RSD 1.2~2.0%), respectively. Liquid chromatography mass spectrometry was used to verify the main components of sodium iron chlorophyllin which were Fe-isochlorin e4 and Fe-chlorin e4.

• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.211-216
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• 2017

BACKGROUND:This study was conducted to investigate residual organochlorine pesticides (ROCPs) in agricultural soils and crops. Agricultural soil samples and crop samples were collected from 93 cities and counties. METHODS AND RESULTS: Extraction and clean-up for the quantitative analysis of ROCPs were conducted by the modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Recovery and limit of detection (LOD) of ROCPs in agriculturalsoils and crops were 76.5-103.0 and 75.2-93.2%, 0.01-0.08 and $0.10-0.15{\mu}g/kg$, respectively. Detected ROCPs in agricultural soils were ${\alpha}$-endosulfan, ${\beta}$-endosulfan, and endosulfan sulfate, the residue were 2.0-12.0, 1.2-53.1, and $2.2-329.8{\mu}g/kg$, respectively. But these pesticides in all green perilla leaf and green pepper samples were not detected. CONCLUSION: These results showed that ROCPs residues in agricultural soils were not as high as crop safety threatening.