• Journal of Food Hygiene and Safety
• /
• v.38 no.5
• /
• pp.297-304
• /
• 2023

Domoic acid (DA), a neurotoxin produced naturally by diatoms, is responsible for incidents of amnesic shellfish poisoning. In this study, a modified analytical method was established to determine domoic acid in seafood using solid phase extraction cleanup and optimizing the amount of sample and extraction solvent to reduce interference effects. The modified method using high-performance liquid chromatography with ultraviolet detection was validated using three seafood matrices (mussel, red snow crab, and anchovy) at three concentrations (1, 2, and 4 mg/kg) and compared to the Food Code method. Compared to the Food Code method, the modified method showed better performance in terms of linearity (R²>0.999), detection limit (0.02-0.03 mg/kg), quantification limit (0.05-0.09 mg/kg), intra-/inter-day accuracy (86.2-100.4%), and intra-/inter-day precision (0.2-4.0%). Furthermore, the method was successfully applied for the analysis of 87 seafood samples marketed in Korea, and DA was detected at a low concentration of 140 ㎍/kg in one anchovy sample. These results suggest that the modified method can be used for routine determination of DA in seafood.

• Korean Journal of Food Science and Technology
• /
• v.42 no.3
• /
• pp.263-268
• /
• 2010

This research was conducted to evaluate the occurrence of ochratoxin A (OTA) in coffee and fruit products in Korea. A total of 388 coffee and fruit product samples were collected from retail or outlet markets; 177 samples were coffee and 211 were fruits or their products. Analytical methods including AOAC and Comit$\acute{e}$ Europ$\acute{e}$en de Normalisation (CEN) were selected and modified by method validation to detect and quantify the OTA in samples. All samples were analyzed by liquid chromatography with fluorescence detection. OTA was detected in 3.9% of 177 kinds of coffee and 0% of 211 kinds of fruit products. The levels of OTA were $0.7-4.6\;{\mu}g/kg$ in green coffee, $0.3-4.8\;{\mu}g/kg$ in roasted coffee, $1.4\;{\mu}g/kg$ in mixed coffee, and $0.4-0.6\;{\mu}g/kg$ in instant coffee. However, OTA was not detected in liquid coffee, dried fruits, or grape juice. OTA levels of all samples detected were less than the European Union legislation of $5.0\;{\mu}g/kg$ in coffee, $10.0\;{\mu}g/kg$ in raisins and $2.0\;{\mu}g/kg$ in grape juice. Therefore, the risk of OTA in coffee and fruit products in Korea is relatively low at safe levels.

• Journal of Food Hygiene and Safety
• /
• v.20 no.4
• /
• pp.244-252
• /
• 2005

This study was performed far development of new analytical method of beet red in foods. In this study, analysis of beet red in foods has been carried out by detection of betanine and isobetanine, the main color component of beet red as indicator compounds. The qualitative analysis technique consisted of clean-up of the colors with a $C_{18}$ cartridge, separation of the colors by cellulose TLC plate using acetone:3-methyl-1-butanol:distilled water (7:7:6) as a solvent system. Also, the quantitative analysis was performed using X-terra RP at wavelength 538 nm and $0.1\%$ phosphoric acid : methanol (90:10) as a solvent. The quantitative results of beet .ed were as follows:900.22$\∼$27701.60 $\mu$g/g for 60 item in nutrient supplement food, $21.95\∼713.40{\mu}g/g$ for 30 items and N.D. for 18 items in cindy, and $155.85{\∼}505.37{\mu}g/g$ for 12 items in ice creams, $43.52\∼64.75{\mu}g/g$ for 18 items and N.D. for 54 item in sauce, N.D. for 12 items in retort food.

• Korean Journal of Food Science and Technology
• /
• v.43 no.5
• /
• pp.544-552
• /
• 2011

The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.

• Korean Journal of Food Science and Technology
• /
• v.31 no.4
• /
• pp.945-951
• /
• 1999

A simple and practical method for the determination of gardenia yellow in foods was developed. In this method, analysis of gardenia yellow in food products has been carried out by the detection of crocetin and/or geniposide as indicator compounds. As a new analytical method for gardenia yellow, we adopted crocetin, which is produced from colored components of gardenia yellow by alkaline hydrolysis, as an indicator compound. The analysis of gardenia yellow was performed by reverse phase high performance liquid chromatography using a Capcell pak $C_{18}$ column at wave length 240 nm (geniposide) and 435 nm (crocetin). The recovery rates of geniposide and crocetin were found to be 93.4% and 87.8% for Dan Mu Ji, 90.2% and 85.9% for milk, 92.8% and 86.5% for snack, respectively. With this method, the range of crocetin and geniposide contents $({\mu}g/g)$ were as follows: $ND{\sim}1.7$ and $ND{\sim}14.1$ for Dan Mu Ji, $ND{\sim}0.2$ and $ND{\sim}13.6$ for milk, $ND{\sim}1.6$ and $ND{\sim}0.9$ for snack, respectively. The detection limits of crocetin and geniposide were 0.07 ${\mu}g/g$ and 0.05 ${\mu}g/g$, respectively.

• Journal of Food Hygiene and Safety
• /
• v.24 no.1
• /
• pp.56-62
• /
• 2009

Patulin, a mycotoxin mainly produced by Penicillium and Aspergillus, is found in various foods. In the present, a maximum acceptable level for patulin is established at $50{\mu}g/kg(ppb)$ in apple juices and apple concentrates in Korea. But patulin may be detected in foods produced with other fruits. In the present study, patulin contamination was analyzed in 520 samples of fruit juices and beverages, and 50 samples of fruit juice concentrates. High performance liquid chromatography(HPLC) was applied to quantitatively analyze patulin levels in samples and liquid chromatography-mass spectrometry(LC/MS/MS) was used to remove false positive results. The results showed that three samples of 520 fruit juices and beverages and five samples of 50 fruit juice concentrates were contaminated by patulin, $9.8-18.0{\mu}g/kg$ and $4.7-18.2{\mu}g/kg$ respectively. Contaminated samples were produced with apple, orange or pear. This indicates that it is necessary to extend the regulatory range of patulin. In the other hands, the present study confirmed the effectiveness of LC/MS/MS analytical method to remove false positive results.

• Journal of Food Hygiene and Safety
• /
• v.32 no.5
• /
• pp.381-388
• /
• 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 fish pathology
• /
• v.18 no.1
• /
• pp.67-80
• /
• 2005

Phosphoinositide-specific phospholipase $C\delta$ $PLC\delta$) plays an important role in many cellular responses and is involved in the production of second messenger. The present study was conducted to obtain the biochemical characteristics of the expressed recombinant $PLC\delta$ in E. coli cloned from Misgurnus mizolepis and partially purified $PLC\delta$ enzymes from liver tissues of M. mizolepis (wild ML-$PLC\delta$). The ML $PLC\delta$ gene was cloned and expressed under the previous report (Kim et al., 2004), and purified the recombinant protein by successive chromatography using $Ni^{2+}$-NTA affinity column and gel iltration FPLC column. The wild ML-$PLC\delta$ protein was solublized with 2 M KCI and purified by successive chromatography on open heparin-Sephagel and analytical TSKgel heparin-5PW. Both the recombinant and wild ML-$PLC\delta$ form of protein showed a concentration-dependent PLC activity to phosphatidylinositol 4,5-bis-phosphate (PIP$_2$) or phosphatidylinositol (PI). Its activity was absolutely $Ca^{2+}$- dependant, which was similar to mammalian $PLC\delta$ isozymes. Maximal PI-hydrolytic activations of recombinant and wild ML- TEX>$PLC\delta$ was at pH 7.0 and pH 7.5, respectively. In addition, the enzymatic activities of recombinant and wild ML-$PLC\delta$ were increased in concentration-dependent manner by detergent, such as sodium deoxycholate SDC), phosphatidylethanolamine (PE) and phosphatidylcholine (PC). The activities decreased in contrast by a polyamine, such as spermine. Western blotting showed that several types of $PLC\delta$ isozymes exist in various organs. Taken together our results, it suggested that the biochemical characteristics of ML-$PLC\delta$ are similar with those of mammalian $PLC\delta1$ and ${\delta}3$ isozymes.

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

• Journal of Food Hygiene and Safety
• /
• v.33 no.3
• /
• pp.176-184
• /
• 2018

The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.