• Analytical Science and Technology
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• v.32 no.1
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• pp.24-34
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• 2019

The safety of food is occasionally questionable, as there have been some reports of products contaminated with illegal adulterants. In this study, the presence of 16 sedative-hypnotics and sleep inducers in dietary supplements was determined by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS). The UPLC method was validated, providing a linearity (R2) of more than 0.999, and LODs and LOQs that ranged from 0.2 to 0.5 and 0.6 to $1.5{\mu}g\;mL^{-1}$, respectively. The repeatabilities were 0.2-8.4 % (intra-day) and 0.3-4.5 % (inter-day), and the accuracies were 89.0-117.0 % (intra-day) and 87.8-111.9 % (inter-day). The mean recoveries of the spiked samples ranged from 98.7 to 107.3 %. The relative standard deviation (%RSD) of the stability was less than 2.4 %. Using the developed method, one sedative-hypnotic compound, phenobarbital, was detected in one of the nineteen samples tested. In addition, the major characteristic fragment ions of each target compound were confirmed using Q-Orbitrap-MS for higher accuracy. Monitoring the presence of these 16 sedative-hypnotics and sleep inducers in dietary supplements should be pursued in the interest of human health, and the results of this study confirmed that the developed method has value for this application.

• Journal of Food Hygiene and Safety
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• v.28 no.2
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• pp.188-193
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• 2013

Anatoxin-a, saxitoxin and neosaxitoxin are produced by Aphanizomenon flos-aquae that is a sort of the cyanobacteria phylum. Therefore, it is not permitted for food materials in Korea. Traditionally, the classification of cyanobacteria has been based on morphological characters such as trichome width, cell size, division planes, shape, and the presence of character such as gas vacuole. But, some diagnostic features, such as gas vacuole or akinetes, can show variation with different environmental or growth conditions and even be lost during cultivation. Therefore, we developed detection method for functional foods containing Aph. flos-aquae by PCR. To design the primer, 16S rRNA region of Aph. flos-aquae, Spirulina laxissima, and Spirulina spp. registered in the GeneBank (www.ncbi.nlm.nih.gov) have been used and for comparative analysis, BioEdit ver. 7.0.9.0. was used. As a result, we was design AFA-F1/AFA-R1 (363 bp) primer for the differentiation Aph. flos-aquae from chlorella, spirulina, green tea, and spinach. Also, it could be distinguished chlorella and spirulina products those are made to contain 1% Aph. flos-aquae.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.327-334
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• 2016

This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.13-21
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• 2019

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination $(R^2){\geq}0.9906$, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

• Journal of Food Hygiene and Safety
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• v.33 no.4
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• pp.266-271
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• 2018

The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

• Korean Journal of Environmental Agriculture
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• v.40 no.2
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• pp.108-117
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• 2021

BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C₁₈ showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides in Korea.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.30-39
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• 2019

An analytical method was developed for the determination of sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reaction monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges ($0.001-0.25{\mu}g/mL$) into a blank extract with $r^2$>0.99. For validation, recovery tests were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedaxane determination in agricultural commodities.

• Journal of Microbiology and Biotechnology
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• v.33 no.2
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• pp.219-227
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• 2023

Lettuce is one of the most consumed vegetables worldwide. However, it has potential risks associated with pathogenic bacterial contamination because it is usually consumed raw. In this study, we investigated the changes in the bacterial community on lettuce (Lactuca sativa L.) in Chungcheong-do, South Korea, and the prevalence of foodborne pathogens on lettuce in different seasons using 16S rRNA gene-based sequencing. Our data revealed that the Shannon diversity index showed the same tendency in term of the number of OTUs, with the index being greatest for summer samples in comparison to other seasons. Moreover, the microbial communities were significantly different between the four seasons. The relative abundance of Actinobacteriota varied according to the season. Family Micrococcaceae was most dominant in all samples except summer, and Rhizobiaceae was predominant in the microbiome of the summer sample. At the genus level, the relative abundance of Bacillus was greatest in spring samples, whereas Pseudomonas was greatest in winter samples. Potential pathogens, such as Staphylococcus and Clostridium, were detected with low relative abundance in all lettuce samples. We also performed metagenome shotgun sequencing analysis on the selected summer and winter samples, which were expected to be contaminated with foodborne pathogens, to support 16S rRNA gene-based sequencing dataset. Moreover, we could detect seasonal biomarkers and microbial association networks of microbiota on lettuce samples. Our results suggest that seasonal characteristics of lettuce microbial communities, which include diverse potential pathogens, can be used as basic data for food safety management to predict and prevent future outbreaks.

• Journal of Radiation Industry
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• v.7 no.1
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• pp.15-21
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• 2013

The detection characteristics of irradiated spices were investigated depending on radiation sources and doses by photostimulated luminescence (PSL) and Thermoluminescence (TL). 6 kinds of spices (turmeric, onion powder, red pepper, basil, parsley, black pepper) were irradiated at 0 to 10 kGy under ambient conditions by both a $^{60}Co$ gamma irradiator and an electron beam (EB) accelerator, respectively. The PSL analysis showed negative results for non-irradiated spices, while irradiated spices gave intermediate and positive value, which presented the limited potential of PSL technique. In TL measurement, TL glow curves on non-irradiated samples appeared at about $300^{\circ}C$ with low intensity. All irradiated samples were easily distinguishable through radiation-specific strong TL glow curves with maximum peak in range of $150{\sim}200^{\circ}C$. TL ratio ($TL_1/TL_2$) obtained by a re-irradiation step could verify the detection result of $TL_1$ glow curves, showing ratios lower than 0.1 in the non-irradiated sample and higher than 0.1 in irradiated ones. Therefore, in PSL measurement, the identification of irradiated spices showed more clear results in electron beam irradiated samples. TL analysis showed obvious difference between non-irradiated and irradiated samples in gamma ray and electron beam irradiated samples.

• Korean Journal of Environmental Agriculture
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• v.32 no.1
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• pp.70-77
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• 2013

BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.