• Korean Journal of Food Science and Technology
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• v.42 no.5
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• pp.541-548
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• 2010

In this study, contamination levels of 7 N-nitrosamine were investigated in processed meat products (n=51), processed fish products (n=62), salted fish pickles (n=20), and beer and malt beverages (n=21) using a GC/PCI-MS/MS method. The limits of detection (LOD) of the N-nitrosamines ranged from 0.2 to 0.5 ${\mu}g$/kg. In addition, methods were used to estimate the recovery of 7 N-nitrosamines, which ranged from 84 to 112%. N-nitrosamines were detected in 89 (58%) out of 154 samples. The exposure of an entire population group to N-nitrosamines through food intake was estimated using the average body weight of the total population and average daily food consumption, to perform risk assessment based on reports of a national health and nutrition survey. The results indicated that the daily intake of N-nitrosamines over a life time was $4.92{\times}10^{-7}$ mg/kg b.w./day. The margin of exposure (MOE) for the general population, estimated using the benchmark dose lower confidence limit 10 ($BMDL_{10}$) of N-nitrosodimethylamine, was 208,939, which was found to be safe.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.53 no.2
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• pp.224-232
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• 2008

The health benefits associated with tea consumption have resulted in the wide inclusion of green tea extracts in botanical dietary supplements, which are widely consumed as adjuvants for complementary and alternative medicines. Tea contains polyphenols such as catechins or flavan-3-ols including (-)-epicatechin (EC), (-)-epigallocatechin (EGC), (-)-epicatechin gallate (ECG), and (-)-epigallocatechin gallate (EGCG), as well as the alkaloid, caffeine. The contents of catechins and caffeine in green tea are considered as a standard of quality evaluation of green tea. Therefor, the purpose of this study was to investigate the most suitable HPLC condition for simultaneous determination of catechins and caffeine in green tea extracts. The efficient HPLC analytical condition of catechins and caffeine contained green tea extracts was developed. The gradient elution employed a $250\;mm\;{\times}\;4.6\;mm$ i.d. YMC-pak ODS-AM 303 column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of 0.1% aqueous phosphoric acid, and mobile phase B, comprising 100% MeOH, and delivered at a flow rate of 1 mL/min as follows: $0{\sim}25\;min$, 80% A; $26{\sim}50\;min$, $80{\sim}70%$ A; 51 min, 80% A. $51{\sim}55\;min$, 80% A. The UV detection wavelength was set at 280 nm. The limit of detection (LOD) for catechins and caffeine standards were under 50 ng/mL.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.303-308
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• 2015

BACKGROUND: Recently, various rice by milling degree is sold for health and taste. To provide safe food to consumers, it is need to know the change of heavy metal contents according to milling degree of rice.METHODS AND RESULTS: This study was to investigate residual the levels of cadmium (Cd), lead (Pb), copper (Cu) and zinc (Zn) as stated in the milling degree of the rice contaminated Cd and Pb from 2011 to 2012 in Chungcheongnam-do. Rice samples exceeded the maximum residue limits (MRL) of Cd and Pb were milled by five degrees (0.0, 2.45, 8.02, 10.48, 15.09%). Milled rice was digested by microwave method, and analyzed heavy metal contents using ICP-OES. Recovery ratios of 4 heavy metals such as Cd, Pb, Cu and Zn were ranged for 79.7-98.9%, and limits of detection (LOD) and limits of quantitation (LOQ) were fulfilled with the normal analytical standards. Concentrations of Cd, Pb, Cu and Zn were ranged 0.416-0.433 mg/kg, 0.183-0.26 mg/kg, 3.639- 3.882 mg/kg and 16.868-19.801 mg/kg, respectively.CONCLUSION: From these results, conforming with increase of milling degree of rice, Cd, Pb, Cu, and Zn contents tended to decrease. The contents of heavy metals were decreased 3.1% in Cd, 29.3% in Pb, 6.4% in Cu and 15.1% in Zn, in according to the highest milling degree of 15.09%.

• Journal of Food Hygiene and Safety
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• v.25 no.2
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• pp.100-105
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• 2010

This study was conducted to establish a method to analyze azodicarbonamide (ADA) in wheat flour. A new method using high performance liquid chromatography (HPLC) was developed for the determination of ADA in wheat flour. The recovery rate was 91.93~97.54%. The limit of detection for ADA was 0.02 mg/kg and the limit of quantification was 0.05 mg/kg. The monitoring results for ADA contents using the established methods showed that it was detected as the low value of 0.95 mg/kg in one of 51 flour samples (detection rate : 2%), but not detected in 59 bakery samples. The detected ADA level was suitable to its usage standard, compared to the standard (45 mg/kg). Although the detection rate was very low, the established analytical method of ADA will contribute to the management of ADA in processed foods such as wheat flour and bakery.

• Food Science of Animal Resources
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• v.28 no.5
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• pp.637-644
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• 2008

Four different extraction and purification methods were evaluated to determine the heterocyclic amines (HCAs) in fried pork patties. Pork patties were cooked in the teflon-coated electric frying pan at $230^{\circ}C$ for 8 min per side. HCAs in the fried pork patties were extracted and purified using four different solid-phase extraction (SPE) methods and quantitated by LC-MS (API-ESI). Recovery of four different extraction and purification methods was evaluated by comparing the HCAs amounts quantified by the standard addition method. Validation of extraction and purification methods for fried pork patties was determined to establish accurate sample preparation. The recoveries of HCAs from different SPE methods were calculated. The recovery yields were 15.7-68.7% (Polar amine group) and 25.0-74.7% (less-polar amine group) in method A. Method D provided recovery yields ranging from 14.1% to 68.7% in polar amine groups and from 3.0% to 72.3% in less-polar amine groups, respectively. Modified procedures of Method A and D were the most suitable extraction and purification method for HCAs analysis from fried pork patties.

• Food Science and Preservation
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• v.20 no.3
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• pp.429-434
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• 2013

This study was designed to investigate the formation of ethyl carbamate (EC) during the ripening of Maesil with sugar and Soju (19.5~35% alcohol contents) using a homemade method. Maesil, sugar and Soju were purchased at ordinary market in June of 2012. The preparation of sample for analysis was conducted by method of Henry et al. The analysis of GC/MS was used SIM mode (m/z 89, 74, 62). Quantification was performed in terms of the 62 ion and was based on an internal standard procedure. Good linearity was obtained with a regression coefficient ($r^2$ = 0.993). Low detection limits (LOD) was achieved 4.31 ug/kg and recovery for alcohol was 74.8%. During 90 days, fermentation with sugar was not detected EC (under LOQ). 15 days ripened Maesil wine contained EC between non detected~32.7 ug/kg and 90 days ripened Maesil wine was 19.7~87.4 ug/kg. Higher proportion of Maesil and Soju increased EC contents. EC levels were increased 32.7 ug/kg to 87.4 ug/kg in the ratio of Maesil to 35% alcohol-Soju (1:1). In the ratio of Maesil to 35% alcohol-Soju (1:3) was increased non detected to 69.7 ug/kg. After 90 days, Maesil wine was filtered Maesil through a seive and ripened by 180 days to investigate the formation of EC compared with non filtered. Treatment of filtered, EC contents was much higher level compared with non filtered. Therefore, this result showed that alcohol contents contribute to increase EC formation more than Maesil.

• Journal of the Korean Society of Food Science and Nutrition
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• v.40 no.4
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• pp.565-569
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• 2011

Validation of quercetin as a marker compound in the standardization of Changnyeong onion extract developed for functional health food was attempted by analytical method. The specificity was satisfied with retention time and photo diode array (PDA) spectrum by analysis of quercetin using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve as coefficient of correlation ($R^2$) of 0.9986, and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.2 mg/L and 0.5 mg/L, respectively. Recovery rate test with quercetin concentration of 0.05, 0.075 and 0.1 mg/mL was revealed in the high range of 82.36~95.26%, 82.70~98.24% and 87.91~95.11%, respectively. The intra-day and inter-day precision in quercetin for Changnyeong onion extracts was 0.10~3.28% and 0.96~5.79%, respectively. Therefore, application of quercetin was validated in analytical method as a marker compound in Changnyeong onion extracts.

• YAKHAK HOEJI
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• v.52 no.6
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• pp.419-425
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• 2008

A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

• YAKHAK HOEJI
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• v.57 no.2
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• pp.87-94
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• 2013

An analytical methodology based on solid-space extraction (SPE) with with Bond Elut Certify cartridge (Varian, 130 mg) has been developed for the qualification and quantitation of strychnine in blood. After the elution layer was evaporated, the residue was reconstituted with methanol for GC/MS. Internal standard was used 10 mg/l dextromethorphan. Strychnine is a potent central nervous stimulant and convulsant, and an alkaloid found in seeds of Strychnos nux-vomica. It was used therapeutically to improve circulation and muscle tone in oral or intramuscular doses of 0.05~8 mg. The fatal dose of strychnine for humans is 50~100 mg. A man was found dead lying curled up the corner of the large room in a roof house after the fire fighter opened a locked door inside to put out the fire. The postmortem blood and gastric contents were analyzed for toxicological testing. Strychnine and brucine were detected using GC/MS first in gastric contents extracts. The contents of strychnine was 0.083 mg/l in heart blood, 0.088 mg/l in peripheral blood and 4.0 mg/kg in gastric contents, respectively. Method validation was carried out in terms of linearity, accuracy, precision (intraday, interday) in blood. The assay is linear over 0.05~10 mg/l ($r^2$=0.999). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.02 mg/l (S/N=3) and 0.07 mg/l (S/N=10), respectively. Accuracy (bias%) of strychnine with 0.1, 1 and 10 mg/l was 12.0% (n=6), 9.3% (n=6) and 6.9% (n=6), respectively. Intraday precision (CV%) of strychnine with, 0.1, 1 and 10 mg/l were 6.4%, 10.4%, 1.2% (n=6), respectively. Interday precision (CV%) of strychnine with 0.1, 1 and 10 mg/l over three days were 24.0%, 18.5%, 13.8% (n=18), respectively. Relative recovery with 0.1, 1 and 10 mg/l (in blood) were 114.9%, 99.3% and 87.4% (n=6), respectively. The described method can be applied in forensic toxicology to determine strychnine in blood samples.

• Journal of Dairy Science and Biotechnology
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• v.34 no.3
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• pp.187-191
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• 2016

Biogenic amines have been used as chemical indicators of fermented foods. So far, several chromatography methods have been developed to detect biogenic amines in foods. However, few methods have identified these compound in domestic cheese. We analyzed the biogenic amines (histamine dihydrochloride, tyramine hydrochloride, ${\beta}$-phenylethylamine hydrochloride, putrescine dihydrochloride, cadaverine, spermidine, tryptamine hydrochloride, ethanolamine hydrochloride and butylamine) in cheese by using HPLC. The calibration curves of the biogenic amines were found to be linear over the concentration range of 10-50 ppm with a correlation coefficient of above 0.99. The limit of detection (LOD) and limit of quantitation (LOQ) of the biogenic amines in the given order were 3.7 and 11.3 ppm, 3.4 and 10.4ppm, 3.4 and 10.3 ppm, 4.0 and 12.2 ppm, 3.4 and 10.4 ppm, 3.4 and 10.5 ppm, 3.5 and 10.7 ppm, 4.1 and 12.5 ppm, and 3.4 and 10.4 ppm, respectively. Recovery rates of the biogenic amines in the given order were 112, 104, 93, 108, 91, 102, 101, and 92%, respectively. The findings of this study suggest that HPLC is a suitable method for the determination of biogenic amines, thereby indicating its potential application in the quality control of aging cheese.