• Analytical Science and Technology
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• v.15 no.6
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• pp.534-539
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• 2002

We established an analytical method for the measurement of trace amounts of earthy/musty odorous geosmin (GSM) and 2-methylisoborneol (2-MIB) in water using GC/MS. Water samples were extracted with n-hexane (liquid-liquid extraction, LLE) and the extracts were measured by GC/MS. The extraction yields of the two compounds were tested to be ($87{\pm}8$)% and ($78{\pm}8$)%, respectively. The limits of quantitation (LOQs) of the two compounds by this method were greatly improved to ~0.3 ng/L. The analytical methods were applied to analyze water samples from several rivers in Korea and waters after water treatment processes. The highest levels of geosmin and 2-methylisoborneol in raw water from a river were measured to be ($4.2{\pm}0.4$) ng/L and ($44{\pm}4$) ng/L, respectively. The levels only slightly decreased to ($1.3{\pm}0.1$) ng/L and ($18{\pm}2$) ng/L even after water treatment, indicating that the odorous compounds were not properly removed by the treatment processes.

• Analytical Science and Technology
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• v.29 no.4
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• pp.179-185
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• 2016

An effective analytical method has been developed for the determination of β-blockers(atenolol, metoprolol and propranolol) and 6 β-lactams(amoxicillin, penicillin G, cefaclor, cefadroxil, cephalexin and cephradine) in water samples using two different cartridges. The samples were extracted by solid-phase extraction (SPE) with the usage of polymeric hydrophile-lipophile balance(HLB cartridges) and strong cation-exchange mixed-mode polymeric sorbent (MCX cartridges). A XDB-C₁₈ column(1.8 μm; 3.0 mm × 100 mm) was used for the sufficient chromatographic resolution. The calibration curves showed good linearity with high correlation coefficients (>0.995). The method detection limits (MDL) and the limits of quantification(LOQ) were from 1.1 to 3.9 ng/L and from 5 to 13 ng/L, respectively. The method was applied for the determination of the target compounds in tributaries and raw water of the Han River and these were found at N.D. to 0.209 μg/L.

• Analytical Science and Technology
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• v.24 no.1
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• pp.10-14
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• 2011

This study was performed to compare international analytical methods of bromide and applied to determine bromide in bottled mineral water and raw ground water in Korea. Bromide in water was eluted by 10~50 mM potassium hydroxide (KOH) and determined by ion chromatography-suppressed conductivity detector (IC-CD). Sample was purified with Ba- and H-on-guard cartridge and $0.2\;{\mu}m$ membrane filter. The method detection limit (MDL) and the limit of quantitation (LOQ) of bromide were 0.2 and $0.5\;{\mu}g/L$, respectively. The calibration curve showed good lineality above 0.9993 in the ranges of the $0.5\sim80\;{\mu}g/L$. A correlation coefficient of bromide in ground water and sum of bromide and bromate in bottled mineral water is 0.808.

• Analytical Science and Technology
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• v.26 no.3
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• pp.182-189
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• 2013

The purpose of this research is to separate and quantitate selenium species in some food samples with HPLC-ICP-MS. Cation exchange chromatography showed efficient separation only for inorganic Se species while reversed phase ion pair chromatography showed good separation for both inorganic and organic Se species. $C_8$ column ($Symmetryshield^{TM}\;RP_8$, 3.5 ${\mu}m$, $4.6{\times}150$ mm) was used with optimum condition of 5% methanol mobile phase, 0.05% of nonafluorovaleric acid ion pairing reagent. Five standard Se species of Se(IV), Se(VI), SeCys(selenocystein), SeMet(selenomethionine) and Se-M-C(seleno methyl cystein) were separated successfully under the optimum condition (mobile phase; 5% methanol, ion-pairing reagent; 0.05% nonafluorovaleric acid, flow rate; 0.9 mL $min^{-1}$). To extract Se species, microwave assisted and enzyme-assisted extraction methods were studied. In enzyme-assisted extraction method, protease I for garlic, protease I plus trypsin for pork and mackerel, and protease XIV for tuna showed the best extraction efficiency. With the optimum condition for each sample, it was found that mostly inorganic Se, SeCys and SeMet are present in the sample studied ranging from few ${\mu}g$ $g^{-1}$ to few tens of ${\mu}g$ $g^{-1}$.

• Korean Journal of Food Science and Technology
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• v.48 no.5
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• pp.454-460
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• 2016

In this study, we investigated the possibility of Droplet digital PCR (ddPCR) for detection of foodborne pathogens. ddPCR combines partitioning of PCR reactions into several thousands or millions of individual droplets in a water-oil emulsion, and counting of positive PCR reaction using flow cytometry. Four species of foodborne pathogens, Bacillus cereus, Staphylococcus aureus, Salmonella Typhimurium and Escherichia coli O157:H7, were used to quantify the target sequence with each of the designed primers and double stranded DNA-binding Evagreen dye. All tested foodborne pathogens showed a detection limit ranging from $100fg/{\mu}L$ to $10ng/{\mu}L$. It was concluded that ddPCR could be used to detect very low concentrations of foodborne pathogens from complex food matrices. For multi-detection of target pathogens, we also tested the samples using multiplex ddPCR and obtained successful results.

• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.89-95
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• 2017

A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.114-122
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• 2017

N-nitrosamines can be produced in the process of heating, processing, storage and packaging. Migration specifications for N-nitrosamines exist only for rubber baby bottle nipples, which are regulated by the Ministry of Food and Drug Safety (MFDS). There is no regulation for other food contact substances (FCS) and studies on N-nitrosamines migration from FCS are rather limited. A pilot study showed an increase in N-nitrosamines contents when cooking instant noodles. Thus, the migration from the packaging was suspected and it was necessary to monitor the migration of N-nitrosamines from food packaging materials and to examine the change in N-nitrosamines contents when cooking instant foods. Three N-nitrosamines, NDMA (N-nitrosodimethtlamine), NDEA (N-nitrosodiethylamine), NDBA (N-nitrosodibutylamine), were analyzed in migration test solutions from plastics such as polyethylene, polypropylene and polystyrene, papers and aluminium containers. In all test solutions, N-nitrosamines were detected less than method quantitation limits (MQLs). Food samples were also investigated to ensure that there is no effect from food contact substances when cooking instant foods. In retort sauces such as curry, black soybean sauce and tomato sauce, NDMA concentration was ranged from 0.54 to $3.81{\mu}g/kg$, but there were no significant differences between unheated and heated samples. However, the NDMA contents were significantly increased in most of the instant noodle samples tested when cooked (p < 0.05). No effects from the food contact substances or cooking water was observed. Only when the seasoning powder and noodles were cooked together was NDMA detected. Individual components (noodle, seasoning powder or dried vegetable) or other combinations such as noodles and dried vegetables did not generate N-nitrosamines. Therefore, it is speculated that NDMA may be formed from the precursors in noodles and seasoning powders when they are solubilized in a medium of water.

• Korean Journal of Food Science and Technology
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• v.34 no.3
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• pp.385-389
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• 2002

Analytical method for diethylstibestrol (DES) and zeranol, which are growth promoters, in muscle foods was studied. Through selected ion monitoring analysis by GC-MSD for hormones, $M^+$ 412, 420, 416, and 433 for DES, $D_8DES$, ${\beta}-estradiol$, and zeranol, respectively, were selected for quantitative analysis. Removal of interferences in meat was done by passing the meat through 1 cc of strong anion exchanges resin, Dowex $2{\times}8$, 400 mesh, whereby the recoveries of DES and zeranol were achieved. Recoveries of DES and zeranol were ranged from 85 to 110%, and 75 to 110%, respectively, in meat using $D_8DES$ as an internal standard, while were 82 to 105%, and 65 to 120%, respectively, using ${\beta}-estradiol$ as an internal standard. These results show that both $D_8DES$ and ${\beta}-estradiol$ can be adopted as the internal standard for the analysis of DES and zeranol in muscle foods. Limits of detection of DES and zeranol were 0.05 and 1.0 ng/g, and limits of quantitation were 0.5 and 1.0 ng/g, respectively. The results of this study revealed no DES and zeranol were present in 14 samples of beefs, porks, ducks, chickens, mutiplicated flat fish, and trout.

• Korean Journal of Food Science and Technology
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• v.32 no.5
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• pp.991-996
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• 2000

Enzyme-linked immunosorbent assay was developed for the analysis of soy protein in foods. Competitive indirect ELISA (ciELISA) was established by using specific antibodies against the heat-stable acidic subunits (AS) of glycinin. Soy proteins in each sample used in this study were solublized in the presence of urea and DTT and boiled at $100^{\circ}C$ for 1hr and then were renatured with a cystine-containing solution. After these treatments, each isolated soy protein (ISP) heated at 60, 70, 80, $90^{\circ}C$ for 10 minutes showed almost the same curve as unheated one in the ciELISA. The detection limit of ISP was 0.3 ${\mu}g/mL$. Anti-AS antibodies have very low reactivities less than 0.1% toward non-meat proteins such as skim milk and casein and did not show any reactivities toward egg white powder and ovalbumin. When laboratory-made sausages containing ISP of $0.5{\sim}3%$ were assayed by ciELISA, the mean recovery was about 83% (C.V., 19%). In addition, the average content of soy protein in commercial sausages was 1.27%.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.3
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• pp.342-351
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• 2016

This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.