• The Korean Journal of Pesticide Science
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• v.18 no.2
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• pp.69-78
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• 2014

In the present study, we developed an official individual analytical method for cymoxanil using HPLC/UVD, respectively in different representative crops. Individual analytical methods for these pesticides are not included in the Korea food code. The samples were extracted with acetonitrile, concentrated and partitioned with dichloromethane and saturated sodium chloride solution. For cymoxanil, extracts were concentrated and clean-up through silica gel column chromatography with dicloromethane/acetone (60/40 v/v) and subjected to instrumental analysis. The limit of detection (LOD) for cymoxanil were 0.1 ng and 1 ng respectively and limit of quantitation (LOQ) were 0.02 mg/kg. Recoveries for cymoxail ranged from 79.6~107.6% respectively, at fortification level of 0.02 mg/kg (LOQ), 0.2 mg/kg (10 LOQ) and 1.0 mg/kg (50 LOQ) and the coefficient of variation (CV) was less than 10%, regardless of sample types. These results were further confirmed with LC/MS. The proposed simultaneous analysis method is reproducible and sensitive enough to determine the residues of cymoxanil in the agricultural commodities. According to the validation data and performance characteristics and high sample throughput, the proposed method is suitable for routine application.

• Journal of Dairy Science and Biotechnology
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• v.33 no.2
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• pp.119-127
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• 2015

To date, detection of microbial populations in dairy products has been performed using culture media, which is a time-consuming and laborious method. The recently developed chromogenic media could be more rapid and specific than classical culture media. However, the newly developed molecular-based technology can detect microbial populations with greater rapidity and sensitivity than the classical method involving culture media and chromogenic media. This molecular-based technology could provide various options for monitoring the characterization of different states of bacteria and cells. Thus, it could help upgrade the processing system of the dairy industry so as to maintain the safety and quality of dairy foods. Among the various newly developed molecular-based technologies, flow cytometry can potentially be used for monitoring microbiological populations in the dairy industry if official international standards are available for this purpose. When omics technology would have biomarker identification, it could be regarded as the rapid and sensitive analytical methods. Methods based on PCR, which has become a basic technique in microbiological research, can be developed and validated as alternative methods for quantification of dairy microorganisms. This review discusses methods for monitoring microbiological populations in dairy foods and the limitations of these studies, as well as the need for further research on such methods in the dairy industry.

• Analytical Science and Technology
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• v.36 no.6
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• pp.291-299
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• 2023

The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R²) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

• Korean Journal of Food Science and Technology
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• v.45 no.5
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• pp.537-544
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• 2013

This study was performed to establish method of simultaneous determination of fructose, glucose, and sucrose in honey and commercial vitamin drinks by GC and GC/MS. Optimum chromatographic separation of trimethylsilyl-oxime (TMSO) derivatives by GC was achieved on a DB-5 column. Calibration curves for fructose, glucose and sucrose TMSO derivatives by GC were linear in the range of 50-5000 ${\mu}g/mL$, and their $r^2$ values were 0.9999, The limit of detection and limit of quantification of fructose, glucose, and sucrose were 0.68, 0.47, and 0.53 ${\mu}g/mL$, respectively, and 2.27, 1.58, and 1.77 ${\mu}g/mL$, respectively. Average recoveries of fructose, glucose, and sucrose were 100.5, 101.0, and 99.7%, respectively. When the method was applied to 12 honey samples, the average concentrations of fructose, glucose and sucrose were $42.58{\pm}1.97%$, $27.74{\pm}1.16%$, and $0.79{\pm}0.52%$, respectively. The F/G ratio was $1.53{\pm}0.07$. For fructose and glucose contents, results from the GC analysis were similar to those from the HPLC analysis, but the sucrose content was different for each analysis method. We suggest that the GC method is more suitable than other official analytical methods for simultaneous determination of fructose, glucose, and sucrose in honey.

• Analytical Science and Technology
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• v.28 no.6
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• pp.409-416
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• 2015

ICP-AES has been used in many laboratories due to the advantages of wide calibration range and multi-element analysis, but it may give erroneous results and suffer from spectral interference due to the large number of emission lines associated with each element. In this study, certified reference materials (CRMs) and field samples were analyzed by ICP-AES and HG-AAS according to the official Korean testing method for soil pollution to investigate analytical problems. The applicability of HG-ICP-AES was also tested as an alternative method. HG-AAS showed good accuracies (90.8~106.3%) in all CRMs, while ICP-AES deviated from the desired range in CRMs with low arsenic and high Fe/Al. The accuracy in CRM030 was estimated as below 39% at the wavelength of 193.696 nm by ICP-AES. Significant partial overlaps and sloping background interferences were observed near to 193.696 nm with the presence of 50 mg/L Fe and Al. Most CRMs were quantified with few or no interferences of Fe and Al at 188.980 nm. ICP-AES properly assessed low and high level arsenic for field samples, at 188.980 nm and 193.696 nm, respectively. The importance of the choice of measurement wavelengths corresponding to relative arsenic level should be noted. Because interferences were affected by the sample matrix, operation conditions and instrument figures, the analysts were required to consider spectral interferences and compare the analytical performance of the recommended wavelengths. HG-ICP-AES was evaluated as a suitable alternative method for ICP-AES due to improvement of the detection limit, wide calibration ranges, and reduced spectral interferences by HG.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.318-327
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• 2015

BACKGROUND: Trinexapac-ethyl is a plant growth regulator (PGR) that inhibits the biosynthesis of plant growth hormone (gibberellin). It is used for the prevention of lodging, increasing yields of cereals, and reducing mowing of turf. The experiment was conducted to establish a determination method for trinexapac-ethyl and its metabolites trinexapac in agricultural products using LC-MS/MS.METHODS AND RESULTS: Trinexapac-ethyl and trinexapac were extracted from agricultural products with methanol/ distilled water and the extract was partitioned with dichloromethane and then detected by LC-MS/MS. Limit of detection(LOD) was 0.003 mg/kg and limit of quantification(LOQ) was 0.01 mg/kg, respectively. Matrix matched calibration curves were linear over the calibration ranges (0.01-1.0 mg/L) for all the analytes into blank extract withr²> 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, 50LOQ,n=5). Recoveries of trinexapacethyl and trinexapac were within the range of 73.6-106.9%, 72.7-99.2%, respectively. The relative standard deviations (RSDs) were less than 9.0%. All values were consistent with the criteria ranges requested in the CODEX guideline(CAC/GL 40, 2003).CONCLUSION: The proposed analytical method was accurate, effective and sensitive for trinexapac-ethyl and trinexapac determination and it can be used to as an official method in Korea.

• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.4
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• pp.459-464
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• 2017

Biphenyl is used as an intermediate in the production of crop protection products, a solvent in pharmaceutical production, and as a component in the preservation of citrus fruits in many countries. Biphenyl is not authorized for use and also does not have standards or specifications as a food additive in Korea. National and imported food products are likely to contain biphenyl. Therefore, control and management of these products is required. In this study, a simple analytical method was developed and validated using HPLC to determine biphenyl in food. These methods are validated by assessing certain performance parameters: linearity, accuracy, precision, recovery, limit of detection (LOD), and limit of quantitation (LOQ). The calibration curve was obtained from 1.0 to $100.0{\mu}g/mL$ with satisfactory relative standard deviations (RSD) of 0.999 in the representative sample (orange). In the measurement of quality control (QC) samples, accuracy was in the range of 95.8~104.0% within normal values. The inter-day and inter-day precision values were less than 2.4% RSD in the measurement of QC samples. Recoveries of biphenyl from spiked orange samples ranged from 92.7 to 99.4% with RSD between 0.7 and 1.7% at levels of 10, 50, and $100{\mu}g/mL$. The LOD and LOQ were determined to be 0.04 and $0.13{\mu}g/mL$, respectively. These results show that the developed method is appropriate for biphenyl identification and can be used to examine the safety of citrus fruits and surface treatments containing biphenyl residues.