• Korean Journal of Food Science and Technology
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• v.44 no.3
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• pp.263-268
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• 2012

Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.

• 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 Food Science and Technology
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• v.42 no.1
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• pp.1-7
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• 2010

To revise the dithiocarbamates residue analysis method and survey the residues in agricultural products that were treated with these fungicides in Korea, we purchased 20 types of foodstuffs (rice, potato, cabbage, apple etc.) from markets in five major cities. 236 samples of the purchased foodstuffs were then analyzed for the presence of dithiocarbamates by HPLC/UV and HPLC/APCI-MS. The $R^2$, LOD and LOQ in the range of 0.5-107.3 mg/L were as follows: DCC: y=174.34x+18.315, $R^2=0.9999$, 0.01 mg/L, and 0.04 mg/L; EBDC: y=227.38x-14.715, $R^2=1.0000$, 0.01 mg/L and 0.02 mg/L; PBDC: y=38.46x-21.412, $R^2=0.9999$, 0.04 mg/L, and 0.1 mg/L; ETU: y=52.752x-4.4819, $R^2=0.9998$, 0.02 mg/L and 0.03 mg/L; PTU: y=128.28x+4.4624, $R^2=0.9998$, 0.02 mg/L, and 0.04 mg/L. The levels of DDC, EBDC, PBDC, ETU and PTU in 20 agricultural products fortified to 10.0-107.3 mg/L ranged from 61.7-117.5%, 65.3-110.1%, 61.5-109.6%, 69.3-116.3% and 70.2-97.2%, respectively. Overall, dithiocarbamates were detected in 100 samples and the detection ratio was 42.4%. Among these, only 3 samples (1.3%) of Lycii fructus had residue levels that were above the action limits, while the remaining samples (233 samples) contained levels of dithiocarbamates below the detection limit or below the Korea MRLs (Maximum Residue Limits).

• Journal of Animal Science and Technology
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• v.53 no.2
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• pp.171-176
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• 2011

Two trials at different body weights of Hanwoo heifers (average body weight of 143 and 257 kg, respectively) were conducted to determine crude protein requirements for maintenance (CPm). Six Hanwoo heifers in each trial were used in two 3 ${\times}$ 3 Latin square design with three diets containing three levels of CP, 14 days in each period. In trial 1, the diets were based on 2.8 kg fresh wt./day/heifer timothy hay (LCP) with supplements of either 250 g ground corn and 150 g corn gluten meal (MCP) or 500 g ground corn and 300 g corn gluten meal (HCP). In trial 2, the diets were based on 4.8 kg fresh wt./day/heifer timothy hay (LCP) with supplements of either 350 g ground corn and 250 g corn gluten meal (MCP) or 700 g ground corn and 500 g corn gluten meal (HCP). In trial 1, CP intakes were 236.6, 340.1, and 459.8 g/d for LCP, MCP, and HCP, respectively. Crude protein balances were 0.51, 1.87 and 3.20g/$BW^{0.75}$/d for LCP, MCP, and HCP, respectively. In trial 2, CP intakes were 415.2, 606.9 and 793.0g/d for LCP, MCP and HCP, respectively. Crude protein balances were 0.67, 1.03, 2.99 g/$BW^{0.75}$/d for LCP, MCP, and HCP, respectively. The maintenance requirements for CP from the regression equation between CP intake and CP balance were 4.58g/$BW^{0.75}$/d (trial 1) and 5.02 g/$BW^{0.75}$/d (trial 2) and lower than the value (5.56 g/$BW^{0.75}$/d) adopted by Korean Feeding Standards for Hanwoo (2007).

• Journal of Animal Science and Technology
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• v.53 no.2
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• pp.155-160
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• 2011

Present experiment was carried out to determine maintenance energy requirements for growing Hanwoo steers. Six Hanwoo steers (BW = $180.6{\pm}3.1$ kg) were used in two 3 ${\times}$ 3 latin square design with three different energy intake levels; TDN 1.70 kg (Low), 2.05 kg (Medium), 2.80 kg (High), respectively, based on the Korean Feeding Standards. Each period lasted 18 days including a 14-day adaptation and a 4-day measuring period. The steers were in the head hood chamber system (one cattle per chamber) during each measuring time to measure heat and methane production for 1 day. Dry matter intake was 2,058, 3,256 and 3,881 g/day for Low, Medium and High TDN, respectively. Increase in energy intake did not affect digestibilities of dry matter, crude protein, crude fiber, crude fat, NDF, ADF and nitrogen-free extract. Gross energy intake averaged 180.21, 292.74 and 337.15 kcal/$BW^{0.75}$ for Low, Medium and High TDN, respectively. Energy loss was 28.7% in feces and 2.1% in urine of gross energy intake. Further, energy loss from methane produced during rumen fermentation was 6~8.3%, while body heat loss averaged 34~60%. Intercept of regression equation between ME intake and retained energy indicated that the energy requirement was 109.84 kcal ME/$BW^{0.75}$.

• Korean Journal of Food Science and Technology
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• v.43 no.6
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• pp.702-710
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• 2011

The occurrence of aflatoxins $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits was investigated. Samples were collected from local markets in Seoul and analyzed by rapid resolution liquid chromatography coupled with tandem mass spectrometry using an immunoaffinity column. The chromatography method was validated for assay of aflatoxins using linearity, accuracy, precision and limit of detection and quantification. The linearity in the concentration ranged from 0.10 to $20{\mu}g/kg$ with $R^2$ > 0.9999. Sample recoveries ranged from 71.1 to 97.2% with relative standard deviations below 4.5% for spiking levels from 1 to $10{\mu}g/kg$. The limits of detection ranged between 0.02 and $0.05{\mu}g/kg$ and the limits of quantification ranged between 0.05 and $0.10{\mu}g/kg$. The levels of aflatoxin $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits were $B_1$ 0.10 to $9.94{\mu}g/kg$, $B_2$ 0.08 to $1.54{\mu}g/kg$, $G_1$ 0.04 to $3.21{\mu}g/kg$ and $G_2$ 0.06 to $0.14{\mu}g/kg$.

• Korean Journal of Food Science and Technology
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• v.40 no.1
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• pp.8-14
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• 2008

This study was performed to establish analysis methods, and evaluated for grayanotoxin in domestic/foreign honey and wild honey. The molecular weight of grayanotoxins I, II and III, excluding grayanotoxin III that has been commercialized, were analyzed by LC-MS/MS. Then, the molecular structure of grayanotoxins I and II were analyzed by NMR. A total 111 samples (25 Korean honey, 21 Korean wild honey, 13 Korean honeycomb honey, 44 foreign honey, 8 foreign wild honey) were examined to determined whether or not each sample contained grayanotoxins I, II, and III. The honey samples were mixed with methanol and loaded into a tC18 cartridge, the filtrate was diluted with water, and the mixture was then analyzed by ESI triple-quadrupole LC-MS/MS. Grayanotoxins were only found in the foreign wild honey and were not detected in Korean honey, Korean honeycomb honey, or Korean wild honey. Three of the samples contained grayanotoxin I, II, and III, and one sample contained only grayanotoxins I and III. The lowest level for grayanotoxin I was 3.13 ${\pm}$ 0.00 mg/kg, and the highest level was 12.93 ${\pm}$ 0.01 mg/kg. The levels of grayanotoxin II were 0.84 ${\pm}$ 0.01 mg/kg, 0.92 ${\pm}$ 0.00 mg/kg and 1.08 ${\pm}$ 0.01 mg/kg, respectively. The lowest level of grayanotoxin III was 0.25 ${\pm}$ 0.01 mg/kg and the highest level was 3.29 ${\pm}$ 0.74 mg/kg. Through this study, safety management for foreign wild honey has been enabled.

• Korean Journal of Food Science and Technology
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• v.34 no.2
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• pp.174-179
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• 2002

A simple and sensitive analysis method based on reverse phase (RP) HPCL with flourescence detector was developed for simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE), and their degradation products, $BADGE{\cdot}H_2O$, $BADGE{\cdot}2H_2O$, $BFDGE{\cdot}H_2O$, $BFDGE{\cdot}2H_2O$, $BADGE{\cdot}HCl{\cdot}H_2O$, $BADGE{\cdot}HCl$, $BADGE{\cdot}2HCl$, $BFDGE{\cdot}HCl{\cdot}H_2O$, $BFDGE{\cdot}HCl$ and $BFDGE{\cdot}2HCl$, which were hydrolyzed and chlorinated forms of BADGE and BFDGE, in canned foods and food simulants. These compounds were identified by GC/MSD with $MSTFA-NH_4I-DTE$ derivatization. Recovery study was performed at each 100 ng/mL levels of BPA, BPF, BADGE and BFDGE added to canned foods and food simulants. This method was resulted in recovery of $90{\sim}114%$ with relative standard deviation of $4.1{\sim}7.0%$, detection limits of $6{\sim}11$ ng/mL and quantitation limits of $12{\sim}18\;ng/mL$. Calibration curves were linear with correlatin coefficients of 0.997 for BPF, 0.996 for BPA, 0.9987 for BFDGE, and 0.9989 for BADGE.

• Korean Journal of Food Science and Technology
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• v.34 no.2
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• pp.141-150
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• 2002

Owing to a need for simple extraction and purification for analysis of water soluble vitamins in food samples by RP-HPLC with UV-detector, the methods of bromelain and protease hydrolysis and $C_{18}$ Sep-Pak solid phase extraction were employed. The recoveries of standard water soluble vitamins by the bromelain and protease hydrolysis and $C_{18}$ Sep-Pak solid phase extraction were significantly high compared to AOAC methods in most of vitamins. The contents of pyridoxal determined with protest in the pork was similar, but in the bromelain hydrolysis and AOAC method, was high compared to the results of reference. The niacinamide, thiamin and riboflavin determined with bromelain and protease hydrolysis showed similar values to the results of references. In the potato, pyridoxamine was detected in the AOAC method, which was not detected in the bromelain and protease hydrolysis methods. Pyridoxal contents in the protease hydrolysis and AOAC methods were very similar to the results of references. The recoveries of fortified standard vitamins in food samples were significantly high and accurate compared to those of AOAC methods. The extraction and purification with $C_{18}$ Sep-Pak solid extractor might be considered superior method for the determination of water soluble vitamins in food samples.

• Korean Journal of Food Science and Technology
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• v.32 no.3
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• pp.544-549
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• 2000

This study was performed to compare optimum analytical method for the contents of naturally occurring sulfur dioxide in foods and to investigate the contents of sulfur dioxide in foods in order to provide a fundamental data when distinguish between added and naturally occurring sulfur dioxide. The determination of the contents of sulfur dioxide in foods from the 20 kinds, 180 cases of samples has been analyzed by the optimized Monier-Williams method, modified Rankine method and Acid Distillation/Ion Chromatography. As a result of the study, the contents of naturally occurring sulfur dioxide in foods by the optimized Monier-Williams method showed from 1.02 to 43.87 ppm and highly content of 43.87, 15.37, 11.50, 11.21 and 10.60ppm were observed in garlic, platicodon, green onion, cabbage and onion, the others were less than 10.00ppm. The sulfur dioxide contents in green onion and garlic by modified Rankine method were showed to be 2.87 and 6.14ppm, respectively, the others were detected less than 2.50ppm. The contents of sulfur dioxide by Acid Distillation/Ion Chromatography showed 15.43, 9.82, 5.74, 5.37, 2.14 and 0.49ppm in garlic, cabbage, green onion, onion, potato and apple, respectively and the others were not detected. And the contents of sulfur dioxide in green onion, onion, cabbage and garlic showed higher levels of sulfur dioxide in these foods than the others because of the naturally occurring sulfur containing compounds. The optimized Monier-Williams method, which is the of official analytical method of Korean Food Code, was suitable for monitoring of sulfur dioxide of most foods. Acid Distillation/Ion Chromatography was thought to be adequate for sulfur containing foods such as green onion, onion and cabbage. In order to distinguish between added and naturally occurring sulfur dioxide, it is though to be need of the fundamental data for the contents of sulfur dioxide in sulfite-free foods and continue the investigation for it.