• Journal of the Society of Cosmetic Scientists of Korea
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• v.31 no.4 s.54
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• pp.289-293
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• 2005

Nowadays there are many sun protection cosmetics including organic or inorganic UV filter as an active ingredient. Chemically stable inorganic sunsEreen agents, usually metal oxides, we widely employed in high SPF products. Titanium dioxide is one of the most frequently used inorganic UV filters. It has been used as pigments for a long period of cosmetic history. With the development of micronization techniques, it becomes possible to incorporate titanium dioxide in sunscreen formulations without whitening effect and it becomes an important research topic. However, there are very few works related to quantitations of titanium dioxide in sunscreen products. In this research, we analyzed amounts of titanium dioxide in sunscreen cosmetics by adapting redof titration, reduction of Ti(IV) to Ti(III) and reoxidation to Ti(IV). After calcification of other organic ingredients of cosmetics, titanium dioxide is dissolved by hot sulfuric acid. The dissolved Ti(IV) is reduced to the Ti(III) by adding aluminum metals. The reduced Ti(III) is titrated against a standard oxidizing agent, Fe(III) (ammonium iron(III) sulfate), with potassium thiocyanate as an indicator In order to test accuracy and applicability of the proposed method, we analyzed the amounts of titanium dioxide in four types of sunscreen cosmetics, such as cream, make-up base, foundation and powder, after adding known amounts of titanium dioxide $(1{\sim}25w/w%)$. The percent recoveries of the titanium dioxide in four types of formulations were in the range between 96 and 105%. We also analyzed 7 commercial cosmetic products labeled titanium dioxide as an ingredient and compared the results with those of obtained from ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry), one of the most powerful atomic analysis techniques. The results showed that the titrated amounts were well coincided with the analyzed amounts of titanium dioxide by ICP-AES. Although instrumental analytical methods, ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) and ICP-AES, are the best for the analysis of titanium, it is hard to adopt because of their high prices for small cosmetic companies. It was found that the volumetric method presented here gat e quantitative and reliable results with routine lab-wares and chemicals.

• Korean Journal of Environmental Agriculture
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• v.40 no.4
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• pp.353-358
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• 2021

BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quantitative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were converted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were extracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was decomposed to 2,4,6-T, and then the partitioned ion-associate was finally purified by optimized aminopropyl solid-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (82.1-89.7%). Good reproducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were reasonable (r² > 0.9986) in the range of 0.005-0.5 ㎍/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines required for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.148-157
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• 2019

An optimized analytical method for sodium iron chloriphyllin in foods was established and verified by using high performance liquid chromatography with attached diode array detection. An Inertsil ODS-2 column and methanol-water (80:20 containing 1% acetate) as a mobile phase were employed. The limit of detection and quantitation of sodium iron chloriphyllin were 0.1 and 0.3 mg/kg, respectively, and the linearity of calibration curve was excellent ($R^2=0.9999$). The accuracy and precision were 93.9~104.95% and 2.0~7.7% in both inter-day and intra-day tests. Recoveries for candy and salad dressing were ranged between 93 and 104% (relative standard deviation, (RSD) 0.3~4.3%), and between 83 and 115% (RSD 1.2~2.0%), respectively. Liquid chromatography mass spectrometry was used to verify the main components of sodium iron chlorophyllin which were Fe-isochlorin e4 and Fe-chlorin e4.

• Journal of Food Hygiene and Safety
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• v.34 no.4
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• pp.340-347
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• 2019

We performed a safety survey on residual pesticides in dried agricultural products. A total of 110 samples of dried agricultural products distributed in Gyeonggi-do were analyzed for 263 pesticides according to multi class pesiticide multiresidue method. Ten types of pesticides were detected in 10 samples. Chlorpyrifos was detected in Ricinus communis leaves, chlorpyrifos, hexaconazole, pyridalyl in Chwinamul (wild aster), diniconazole, isoprothiolane, lufenuron in radish leaves, hexaconazole in Cirsium setidens (Korean thistle), bifenthrin, and chlorothalonil, boscalid, and pyraclostrobin in pepper leaves. The detection rate of pesticides was 9.1%, and among these samples, one was detected over Maximum Residue Limits (MRLs). In the validation study, the values of limit of detection (LOD), limit of quantitation (LOQ), coefficient of determination ($R^2$) and recovery were in the range of 0.002~0.027 mg/kg, 0.006~0.083 mg/kg, 0.9964~1.0000 and 74.8~118.9%, respectively. The Positive List System (PLS) was newly introduced as part of the safety management of residual pesticide in agricultural products in Korea in 2019. With the application of the PLS, if the MRL is not established, 0.01 mg/kg limit is applied uniformly. In spite, these of strengthened residue limits, the MRLs of dried agricultural products are still insufficient. Therefore, this study could be utilized as basic data for the setting of proper MRLs.

• 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.191-198
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• 2019

This study investigated the residual characteristics of bifenthrin and chlorothalonil in crown daisy and suggested pre-harvest residue limits (PHRLs) based on their dissipation patterns and biological half-lives. The samples for residue analysis were harvested at 0 (3 hr), 1, 3, 5, 7, 9, 11, 13, 15, 18, 22 and 26 days after treatment, and analyzed by $GC/{\mu}-ECD$ and TOF/MS. The limit of quantitation (LOQs) of bifenthrin and chlorothalonil were 0.0046 mg/kg and 0.0007 mg/kg, respectively. Recoveries ranged from $88.67{\pm}7.97%$ and $99.90{\pm}16.03%$, showing that this method is appropriate for the analysis of the pesticide residues in crown daisy. Being well within first order kinetics, the biological half-lives of the pesticide residues in crown daisy were 9.63 days for bifenthrin and 6.54 days for chlorothalonil. The PHRLs of bifenthrin and chlorothalonil were recommended as 11.70 mg/kg and 24.10 mg/kg for 26 days before harvest, respectively.

• Korean Journal of Agricultural and Forest Meteorology
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• v.24 no.4
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• pp.285-294
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• 2022

In order to accurately calculate greenhouse gas emissions in the agricultural field, Korea has been developing national-specific emission factors through direct measurement of gas fluxes using the closed-chamber method. In the rice paddy, only national-specific emission factors for methane (CH₄) have been developed. It is thus necessary to develop those for nitrous oxide (N₂O) affected by the application of nitrogen fertilizer. However, since the concentration of N₂O emission from rice cultivation is very low, the QA/QC methods such as method detection and practical quantification limits are important. In this study, N₂O emission from a rice paddy was evaluated affected by the amount of nitrogen fertilizer, by taking into account both method detection and practical quantification limits for N₂O concentration. The N₂O emission from a rice paddy soils affected by the nitrogen fertilizer application was estimated in the following order. The method detection limit (MDL) of N₂O concentration was calculated at 95% confidence level based on the pooled standard deviation of concentration data sets using a standard gas with 98 nmol mol^-1 N₂O 10 times for 3 days. The practical quantification limit (PQL) of the N₂O concentration is estimated by multiplying 10 to the pooled standard deviation. For the N₂O flux data measured during the rice cultivation period in 2021, the MDL and PQL of N₂O concentration were 18 nmol mol^-1 and 87 nmol mol^-1, respectively. The measured values above the PQL were merely about 12% of the total data. The cumulative N₂O emission estimated based on the MDL and PQL was higher than the cumulative emission without nitrogen fertilizer application. This research would contribute to improving the reliability in quantification of the N₂O flux data for accurate estimates of greenhouse gas emissions and uncertainties.

• Korean Journal of Environmental Biology
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• v.40 no.3
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• pp.316-324
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• 2022

Ethyl formate (EF) is a potent fumigant replacing methyl bromide. The use of EF is limited to a quarantine process. Appling EF to agricultural field as a safe insecticide in greenhouse give us valuable benefits including less residual concern. In this regard, residual pattern after EF fumigation in greenhouse should be undertaken. In the previous study, we have established agricultural control concentration of EF to control pests in a greenhouse. EF was fumigated at 5 g m^-3 level for 2 h. The concentration of EF inside a greenhouse was analyzed to be 4.1-4.3 g m^-3 at 30 min after fumigation. To prepare an analytical method for residues in cucumber crops and soil in the greenhouse, the limit of detection(LOD) of the method was 100ng g^-1 and the limit of quantitation(LOQ) of this method was 300 ng g^-1. R² values of calibration curves for crops and soil were 0.991-0.997. In samples collected immediately after ventilation, EF concentration was determined to be below LOQ level. In addition, EF level was below LOQ in samples collected at 3 h after ventilation except that leaf samples of melon during the flowering period showed a level of 1,068.9 ng g^-1. Taken together, these results indicate that EF used in quarantine can be applied to agricultural fields without residual issue as an effective fumigant for insect pest control.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.390-401
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• 2023

Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r²=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.319-331
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• 2023

Aminoglycoside antibiotics, also known as aminoglycosides (AGs), are veterinary drugs effective against a wide range of gram-negative and gram-positive bacteria. Owing to their recent use in cultured meats, it has become essential to establish an analytical method for safety management. AGs are highly polar compounds, and ion-pair reagents (IPRs) are used to ensure component separation. Owing to the high possibility of potential mechanical problems resulting from IPR addition to the mobile phase, an analytical method in which IPRs are added directly to the vial was explored. In this study, methods for analyzing 10 AGs via liquid chromatography-tandem mass spectrometry (LC-MS/MS) with the addition of two IPRs were validated for selectivity, detection limit, quantitation limit, recovery, and precision. The detection limit was 0.0001-0.0038 mg/kg, the quantification limit was 0.004-0.011 mg/kg, and the linearity (R²) within the concentration range of 0.01-0.5 mg/kg was over 0.99. Recovery and precision (expressed as relative standard deviation) evaluated in the two matrices (beef and cell culture media) ranged from 70.7% to 120.6% and 0.2% to 24.7%, respectively. The validated AG analytical method was then applied to 15 meats prepared from chicken, beef, and pork, and 6 culture media and additives used in cultured meat. No AGs were detected in any of the 15 meats distributed in Korea; however, streptomycin and dihydrostreptomycin were detected at levels ranging from 695.85 to 1152.71 mg/kg and 6.35 to 11.11 mg/kg, respectively, in the culture media additives. The LC-MS/MS method coupled with direct addition of IPRs to the vial can provide useful basic data for AG analysis and safety evaluation of meats as well as culture media and additives for cultured meats.