• 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.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.424-433
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• 2017

Antioxidants are used in the manufacturing of commercial food packages made of polyolefin plastic such as polyethylene and polypropylene for the purpose to delay the oxidation reaction of the polymer due to oxygen or traces of ozone in the atmosphere. Additives in plastics may be migrated from the packaging materials into foods, thereby presenting a potential health risk to the consumer. Therefore, it is necessary to determine migration level of antioxidants from food packaging materials to foodstuffs in order to take proactive management. In this study, we have developed a method for the analysis of 10 antioxidants, which are butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), Cyanox 2246, 425 and 1790, Irgafos 168, and Irganox 1010, 1330, 3114 and 1076, migrated from the food packaging materials into four food simulants for aqueous, acidic, alcoholic and fatty foods. The antioxidants were determined by reversed-phase high-performance liquid chromatograph-ultraviolet detector with 276 nm after solid-phase extraction with a hydrophilic-lipophilic balance (HLB) cartridge or dilution with isopropanol. The analytical method showed a good linearity of coefficient ($R^2{\geq}0.99$), limits of detection (0.11~0.41 mg/L), and limits of quantification (0.34~1.24 mg/L). The recoveries of antioxidants spiked to four food simulants ranged from 71.3% to 109.4%. The migrated antioxidants in this study were within the safety levels that resulted from the safety assessment by the estimated daily intake to the tolerable daily intake.

• Journal of Food Hygiene and Safety
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• v.31 no.4
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• pp.227-249
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• 2016

Arsenic and its compounds vary in their toxicity according to the chemical forms. Inorganic arsenic is more toxic and known as carcinogen. The provisional tolerable weekly intake (PTWI) of $15{\mu}g/kg$ b.w./week established by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) has been withdrawn, while the EFSA panel suggested $BMDL_{0.1}$ $0.3{\sim}8{\mu}g/kg\;b.w./day$ for cancers of the lung, skin and bladder, as well as skin lesions. Rice, seaweed and beverages are known as food being rich in inorganic arsenic. As(III) is the major form of inorganic arsenic in rice and anaerobic paddy soils, while most of inorganic arsenic in seaweed is present as As(V). The inorganic arsenic in food was extracted with solvent such as distilled water, methanol, nitric acid and so on in heat-assisted condition or at room temperature. Arsenic speciation analysis was based on ion-exchange chromatography and high-performance liquid chromatography equipped with atomic absorption spectrometry and inductively coupled plasma mass spectrometry. However, there has been no harmonized and standardized method for inorganic arsenic analysis internationally. The inorganic arsenic exposure from food has been estimated to range of $0.13{\sim}0.7{\mu}g/kg$ bw/day for European, American and Australian, and $0.22{\sim}5{\mu}g/kg$ bw/day for Asian. The maximum level (ML) for inorganic arsenic in food has established by EU, China, Australia and New Zealand, but are under review in Korea. Until now, several studies have conducted for reduction of inorganic arsenic in food. Inorganic arsenic levels in rice and seaweed were reduced by more polishing and washing, boiling and washing, respectively. Further research for international harmonization of analytical method, monitoring and risk assessment will be needed to strengthen safety management of inorganic arsenic of foods in Korea.

• Food Science and Preservation
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• v.24 no.7
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• pp.983-991
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• 2017

This study was performed to update the National Standard Food Composition Table (NSFCT) published by Korea Rural Development Administration, especially focusing on vitamin $B_{12}$ for Korean pork. Total 7 primal and 22 retail fresh cuts of Korean pork were analyzed for vitamin $B_{12}$ and the applied immunoaffinity-HPLC was validated. Vitamin $B_{12}$ assay by immunoaffinity-HPLC obtained recoveries over 95% and coefficient variations of precision below about 10%, which met the limits required for validation acceptance. Limits of detection and quantification of immunoaffinity-HPLC were 0.01 and $0.33{\mu}g/100g$, respectively. Quality control chart showed that analysis performance was excellent during the entire of study. Vitamin $B_{12}$ contents of pork cuts significantly varied depending the types of primal and its retail cuts (p<0.05). Belly, Boston butt, rib cuts showed relatively high vitamin $B_{12}$ contents compared to other primal cuts. Vitamin $B_{12}$ content of pork retail cuts were also significantly different within the same primal cuts (p<0.05). Among 22 retail cuts, the highest vitamin $B_{12}$ was observed in Tosisal in belly primal part ($0.98{\mu}g/100g$) while both Aldeungsimsal in loin and Hongdukkaesal in hide leg were the lowest by $0.33{\mu}g/100g$. This study provides reliable vitamin $B_{12}$ data for the Korean pork fresh cuts through standard sampling, method validation and analytical quality control, which would be used for update of Korean NSFCT.

• Journal of Life Science
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• v.24 no.3
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• pp.252-259
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• 2014

The leaves of Peatasites japonicus are a traditional oriental medicine with diverse biological activities. A simple and specific analytical method for the quantitative determination of bakkenolide B constituents from methanolic extract of the leaves of P. japonicus was developed. Bakkenolide B was isolated from the leaves of P. japonicus, and its structure was elucidated based on 1D, 2D NMR, and GC-MS spectral data. A liquid chromatographic method was developed to evaluate the quality of P. japonicus through determination of major active compound, bakkenolide B. The wavelengths at 254 and 215 nm were chosen to determine bakkenolide B. The recovery of the method was in the range of 98.6 to 103.1%, and bakkenolide B showed good linearity ($r^2$=0.999) within test ranges. The developed method was applied to the determination of bakkenolide B in the plant part and seasonal changes. The results showed that the content of bakkenolide B in the leaf was higher than in the petiole and rhizome. In this study, a simple, rapid, and reliable high-performance liquid chromatography method was used to determine the percentage and composition of bakkenolide B in P. japonicus procured from different Petasites species plants in South Korea. The method can be employed in routine quantitative analysis and quality control of different products in the market.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.11
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• pp.1666-1671
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• 2015

The purpose of this study was to provide trustworthy nutritional information by analyzing sugar contents of commercial retort foods. A total of 70 retort food samples were collected, which included curry (n=21), blackbean- sauce (n=16), sauce (n=17), and meat (n=16) from markets in Seoul and Gyeonggi-do. Contents of sugars such as glucose, fructose, sucrose, maltose, and lactose were analyzed in retort foods by using a high performance liquid chromatography-refractive index detector and compared to their assigned values on nutritional information labels. Analyzed sugar contents of curries, black-bean-sauces, sauces, and meats ranged from 1.05~4.63 g/100 g, 1.76~5.16 g/100 g, 0.35~25.44 g/100 g, and 1.98~11.07 g/100 g, respectively. Sauces were found to contain the highest amounts of total sugar. These analysis values were equivalent to the reference values indicated on nutrition labels, which were 40~119.5% for curries, 29~118% for black-bean-sauces, 18~118% for sauces, and 70~119.8% for meats. Therefore, this study provides reliable analytical values for sugar contents in retort foods.

• Korean Journal of Food Science and Technology
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• v.41 no.4
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• pp.458-463
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• 2009

To establish and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the rapid and accurate quantitation of diarrhetic shellfish poisoning (DSP) toxins, we compared the results from different mobile phases and columns used for their analysis and collision energies for MS/MS experiments. Clear peaks of okadaic acid (OA) and dinophysistoxin-1 (DTX1) were obtained by using a mobile phase comprising aqueous acetonitrile containing 2 mM ammonium formate and 50 mM formic acid. The collision energies were optimized to facilitate the most sensitive detection for each toxin, namely, OA, DTX1, pectenotoxin-2 (PTX2), or yessotoxin (YTX). Further, the maximum ion response was obtained at a collision energy of 48 V for OA and DTX1. We compared the analytical performance of $C_8$ and $C_{18}$ columns. A wide range of toxins namely, OA, DTX1, PTX2, and YTX, except DTX3, were detected by both the columns. Although DTX3 was only detected by the $C_8$ column, we found that the $C_{18}$ column was also suitable for the quantitation of OA and DTX1 the toxins responsible for inducing diarrhea. The limit of detection of OA and DTX1 by the established LC-MS/MS conditions was 1 ng/g, and the limit of quantitation of the toxins under the same conditions was 3 ng/g. The process efficiencies were 91-118% for oysters (Crassostrea gigas) and 96-117% for mussels (Mytilus galloprovincialis) further, we observed no significant effect of matrix during the ionization process in LC-MS/MS. The comparison between mouse bioassay (MBA) and LC-MS/MS yielded varying results because low concentrations of OA and DTX1 were detected by LC-MS/MS in some shellfish samples, which provided positive results on MBA for DSP. The analysis time required by MBA for DSP analysis can be reduced by LC-MS/MS.

• The Korean Journal of Pesticide Science
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• v.19 no.1
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• pp.5-13
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• 2015

A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

• Journal of Korean Society of Steel Construction
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• v.23 no.4
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• pp.417-428
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• 2011

Depending on the plastic deformation capacity required, structural steel design under the current codes can be classified into three categories: elastic, plastic, and seismic design. Most of the current steel codes explicitly forbid the use of a steel material with a yield strength higher than 450 MPa in the plastic design because of the concerns about its low plastic deformation capacity as well as the lack of test data on local and lateral torsional buckling behavior. In this study, flexural tests on full-scale H-shape members built with SM490A (ordinary steel or benchmark material) and HSB800 (high-strength steel) were carried out. The primary objective was to investigate the appropriateness of extrapolating the local buckling criterion of the current codes, which was originally developed for normal-strength steel, to the case of high-strength steel. All the SM490A specimens performed consistently with the current code criteria and exhibited sufficient strength and ductility. The performance of the HSB800 specimens was also very satisfactory from the strength perspective; even the specimens with a noncompact and slender flange developed the plastic moment capacity. The HSB800 specimens, however, showed an inferior plastic rotation capacity due to the premature tensile fracture of the beam bottom flange beneath the vertical stiffener at the loading point. The plastic rotation capacity that was achieved was less than 3 (or the minimum level required for a plastic design). Although the test results in this study indicate that the extrapolation of the current flange local-buckling criterion to the case of high-strength steel is conservative from the elastic design perspective, further testing together with an associated analytical study is required to identify the causes of the tensile fracture and to establish a flange slenderness criterion that is more appropriate for high-strength steel.

• Korean Journal of Food Science and Technology
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• v.33 no.5
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• pp.641-644
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• 2001

This study was performed for development of new analytical method of monascus pigments in foods. In this method, analysis of monascus pigment in foods has been carried out by detection of monascin and ankaflavin of the main color component of monascus pigment as indicator compounds. Monascin and ankaflavin were isolated and identified by TLC, HPLC, Prep. HPLC, $^{1}H-NMR$ and Mass spectrophotometer. The analysis of monascin and ankaflavin in foods such as massal, sausage, mixed press ham, mixed fish sausage, semi-dried sausage and syrup was performed by using reverse phase high performance liquid chromatograph with Capcell Pak C18 column at wave length 390 nm. The quantitative results of monascin were as follows : $0.01{\sim}3.31\;{\mu}g/g$ item in massal, $0.05{\sim}0.10\;{\mu}g/g$ in mixed fish sausage, and $0.34{\sim}0.35\;{\mu}g/g$ in semi-dried sausage. But the quantitative results of ankaflavin were as follows: $0.02{\sim}0.89\;{\mu}g/g$ in massal, ankaflavin were not founded in other samples.