• KOREAN JOURNAL OF CROP SCIENCE
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• v.64 no.4
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• pp.452-458
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• 2019

Coix lacryma-jobi var. ma-yuen (Rom. Caill.) Stapf (CL), which contains riboflavin and coixol, has traditionally been used to treat cancer and arthritis. However, no method for the simultaneous determination of riboflavin and coixol in CL sprouts has been established. In this study, we established and validated a high-performance liquid chromatography-diode array detection (HPLC-DAD) method for the identification and quantification of two reference markers, riboflavin and coixol, in CL sprout extracts. CL sprouts (whole sprouts and leaves) were subjected to extraction with 70% ethanol at room temperature and at 80 ℃ under reflux conditions. The two extractions were validated with respect to specificity, accuracy, precision, and linearity. The content of the two reference markers was highest in leaves extracted under reflux conditions (riboflavin, 8.23 ± 0.32 mg/g; coixol, 5.95 ± 0.04 mg/g). We also investigated the antioxidant activity of the extracts via 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS⁺) scavenging assays. The results indicated that extracts obtained from sprouts under reflux conditions had the strongest antioxidative effects (DPPH half maximal inhibitory concentration [IC₅₀], 68.9 ± 4.1 g/mL; and ABTS, IC₅₀, 34.9 ± 0.1 g/mL). These results can serve as baseline data for the simultaneous determination of the two reference marker compounds, riboflavin and coixol, and development of functional food materials using CL sprouts.

• Korean Journal of Poultry Science
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• v.43 no.2
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• pp.111-118
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• 2016

Mycotoxins are secondary metabolites produced by molds, such as Aspergillus, Fusarium and Penicillium, that have adverse effects on animals and humans. Aflatoxin, ochratoxin, zearalenone, fumonisin and deoxynivalenol are the mycotoxins of greatest agro-economic importance and cause acute disease called mycotoxicoses. Mycotoxicosis in poultry birds results in decreased meat/egg production, immunosuppressant, and hepatotoxicosis. Some of toxins or their metabolites may be retained in animal or human tissues and induce health problems. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of mycotoxins, such as aflatoxin $B_1$, aflatoxin $M_1$, ochratoxin A, zearalenone, fumonisin B and deoxynivalenol, in chicken liver and kidney tissues. The mycotoxins were extracted and purified using modified QUECHERS methods, separated by LC and detected by an electrospray ionisation interface (ESI) and tandem MS. Good precision and linearity were observed for most of six mycotoxins. The recovery test for each mycotoxin in liver and kidney tissues mostly indicated good average recovery rates between 80.94% and 98.10% and the coefficient of variation mostly under 13.78%, except for aflatoxin $M_1$ and fumonisin $B_1$. The limit of detection (LOD) for six mycotoxins was $7.6{\sim}145.79{\mu}g/kg$ in liver tissues and $6.07{\sim}197.20{\mu}g/kg$ in kidney tissues. The quantification limits (LOQ) for 6 mycotoxins were in the range $23.04{\sim}441.78{\mu}g/kg$ in liver tissues and $18.40{\sim}597.59{\mu}g/kg$ in kidney tissues, respectively. The developed multi-mycotoxin method in this study permits simultaneous, simple, and rapid determination of several co-existing mycotoxins in chicken liver and kidney tissues.

• Korean Journal of Food Science and Technology
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• v.45 no.1
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• pp.111-119
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• 2013

Eleven mycotoxins, including aflatoxins, ochratoxin A, fumonisins, zearalenone, T-2 toxin, deoxynivalenol, and HT-2 toxin, were analyzed simultaneously in rice, barley, and maize produced in 2011 by liquid chromatography coupled with triple quadrupole mass spectrometry (LC/MS/MS). Limits of detection (LOD) are 0.2 ${\mu}g/kg$ for aflatoxin $B_1$, and $G_1$, 0.3 ${\mu}g/kg$ for aflatoxins $B_2$, and $G_2$, 0.1 ${\mu}g/kg$ for ochratoxin, fumonisins, zearalenone, and T-2 toxin and 3.0 ${\mu}g/kg$ for deoxynivalenol and HT-2 toxin. Limits of quantification (LOQ) were 0.6 ${\mu}g/kg$ for aflatoxins $B_1$, and $G_1$, 0.9 ${\mu}g/kg$ for aflatoxins $B_2$, and $G_2$, 0.3 ${\mu}g/kg$ for ochratoxin, fumonisins, zearalenone, and T-2 toxin and 10.0 ${\mu}g/kg$ for deoxynivalenol and HT-2 toxin. Recoveries for 11 mycotoxins ranged from 70.45 to 111.11%. Fumonisins, deoxynivalenol, and zaeralenone were detected from 0.9 to 334.0 ${\mu}g/kg$ in the polished rice, barley and raw corn cultivated in Korea. Other mycotoxins were not detected. Deoxynivalenol contamination was mainly found in barley (24 out of 43 samples) and the average value in positive samples was 113.30 ${\mu}g/kg$.

• Korean Journal of Food Science and Technology
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• v.45 no.1
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• pp.25-33
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• 2013

Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

• Journal of Food Hygiene and Safety
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• v.30 no.3
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• pp.265-271
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• 2015

This study was done in order to investigate the naturally occurring levels of nitrate and nitrite in livestock products. Total samples of 458 consisting of meats (n = 223), processed meat products (n = 51), raw milks (n = 30), processed milk products (n = 142), eggs (n = 5) and processed egg products (n = 7) were analyzed for contents of nitrate and nitrite by ion chromatography (IC). That methods showed good results in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ), recovery, reproducibility and uncertainty. Nitrate and nitrite were detected in 167 and 40 samples, respectively. The nitrate levels (mg/kg) were not detected (ND)~40.23 for modified milks, ND~37.97 for sauce meats, ND~32.40 for process cheeses, ND~31.50 for processed egg products, ND~27.73 for dry milks, ND~24.76 for sausages, ND~22.45 for bacons, ND~21.55 for natural cheeses, ND~20.82 for hams and fermented milks, ND~13.57 for eggs, ND~12.77 for butters, ND~9.31 for milks and ND~3.88 for meats while the nitrite levels (mg/kg) were ND~17.35 for processed egg products and ND~1.92 for meats. In conclusion, the result of this study of nitrate and nitrite in livestock products could be used as one of scientific base datum to determine whether they are naturally occurring or not, including ingredients and their percentage, manufacturing processes, other papers relating to naturally occurring levels of them, and so on.

• Korean Journal of Environmental Agriculture
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• v.37 no.4
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• pp.283-290
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• 2018

BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.

• Journal of Food Hygiene and Safety
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• v.33 no.6
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• pp.466-473
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• 2018

An analytical method of sodium polyacrylate in processed food products was developed and monitored by using size-exclusion chromatography. GF-7M HQ column and UV/VIS detector were selected based on peak shape and linearity. Flow rate, column oven temperature, and mobile phase were selected as 0.6 mL/min, $45^{\circ}C$, and 50 mM sodium phosphate buffer of pH 9.0, respectively. Samples for analysis of sodium polyacrylate were extracted with 50 mM sodium phosphate buffer of pH 7.0 for 3 hr at $20^{\circ}C$ and 150 rpm. Analytical method validation revealed proper selectivity and calibration curve was selected in the range of 50-500 mg/L, and correlation coefficient of calibration curve was more than 0.9985. Limit of detection of sodium polyacrylate was 10.95 mg/kg and limit of quantification was 33.19 mg/kg. Accuracy and coefficient of variation for sodium polyacrylate analysis was 99.6-127.6%, 3.0-8.3% for intra-day and 94.3-121.9%, 1.3-2.6% for inter-day, respectively. Sodium polyacrylate was detected in 40 samples among monitored 125 processed food products. Detected contents were less than 0.2%, limited by the Food Additives Code. Results suggest the established size-exclusion chromatography method could be used to analyze sodium polyacrylate in processed food products.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.65-72
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• 2019

This study was aimed at investigating the levels of the natural preservatives of benzoic, sorbic and propionic acids in cereal grains, nuts and seeds. Benzoic and sorbic acid were analyzed by high-performance liquid chromatography with a diode-array detector (HPLC-DAD) and further confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), whereas propionic acid was analyzed using a gas chromatography-flame ionization detector (GC-FID) and further confirmed by gas chromatography-mass spectrometry (GC-MS). Benzoic, sorbic and propionic acids were found in 44, 22, and 550 samples out of 702 samples, respectively. From the total of 702 samples. The concentrations of benzoic, sorbic and propionic acid were ranged from not detected (ND) to 23.74 mg/L, from ND to 7.90 mg/L, and from ND to 37.39 mg/L in cereal grains, nuts and seeds, respectively. The concentration ranges determined in this study could be used as standard criteria in the process of inspecting cereal grains, nuts and seeds for preservatives as well as to address consumer complaints or trade disputes.

• Korean Journal of Food Science and Technology
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• v.51 no.4
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• pp.316-323
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• 2019

It is difficult to analyze pymetrozine in citrus fruits using the hydromatrix method because of its low efficiency of purification and overlap of matrix and pymetrozine peaks. Liquid-liquid extraction can analyze pymetrozine in citrus fruits using dichloromethane. Since low pH interferes with the extraction of pymetrozine, the extracts of citrus fruits were maintained over pH 7.0 by adding borax buffer and 1 N NaOH in the improved method. According to the improved method, citrus fruits (such as lemon, lime, orange, tangerine, and grapefruit) were extracted and purified for HPLC-photo diode array analysis. The results of validation were as follows: $4.360{\mu}g/kg$ of limit of detection, $14.533{\mu}g/kg$ of limit of quantitation, and 0.007 mg/kg of method quantitative limit. Citrus fruits spiked with pymetrozine showed a recovery range from 71.8 to 83.7% and a coefficient of variation below 6%. Thus, the improved method can efficiently analyze pymetrozine in citrus fruits.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.158-169
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• 2019

Ergot alkaloids are mycotoxin produced by fungi of the Claviceps genus, mainly by Claviceps purpurea in EU. Recently obtained informations indicates necessity for control the ergot in imported grains. Recent occurrence data of ergot alkaloids from EU countries indicate the necessities of management and control these toxins from the imported grains like rye, wheat, oat etc. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine and their epimers (-inines) from grain and grain-based food. The test method was optimized by extracting the sample with acetonitrile containing 2 mM ammonium carbonate, purification with Mycosep cartridge, and instrumental analysis by LC-MS/MS using Syncronis C18 column. The standard calibration curves showed linearity with correlation coefficents; $R^2$ >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and $100{\mu}g/kg$). The correlation coefficient expressed as precision was within the range of 1.9-12.9%. The limit or quantifications (LOQ) ranged from 0.012 to $0.058{\mu}g/kg$. The developed analytical method met the criteria of AOAC Int. and CAC validation parameters like accuracy and sensitivity. As a result, it was confirmed that the test method developed in this study is suitable for the simultaneous analysis of six species of ergot alkaloid from grains and grain products.