• 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.

• Korean Journal of Environmental Agriculture
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• v.41 no.2
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• pp.82-94
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• 2022

BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO₄, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C₁₈) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO₄. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.124-134
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• 2019

An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

• The monthly packaging world
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• s.281
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• pp.98-100
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• 2016

식품의약품안전처는 의약품 투약계량기의 기준 및 시험방법을 대한민국약전 이외에 식품의약품안전처장이 정하는 공정서 및 의약품집을 따를 수 있도록 하고, 규정된 시험방법보다 정확도와 정밀도가 더 좋은 시험방법이 있는 경우 규정된 시험방법을 대신해 시험할 수 있도록 하는 등 의약품 투약계량기의 시험방법을 합리적으로 운영하기 위해 의약품 안전용기 포장 및 투약계량기에 관한 규정 일부개정고시안을 행정 예고했다. 다음에 주요내용과 신 구조문대비표 등에 관해 살펴보도록 한다.

• Food Science and Industry
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• v.49 no.2
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• pp.8-17
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• 2016

Sodium is a component of salt and naturally taken in the process of taking in table salt. For food processing, salt is very important. In general, salt adds flavor and taste including a salty taste and rheologically, it plays an important role in forming tissues. Also, it helps in improving preservability of food by controling growth of microorganisms. But excessive intake of salt has been blamed for outbreak of high blood pressure, heart disease, stroke, osteoporosis, kidney stone, stomach cancer and others. For this reason, there are active efforts to reduce sodium of processed foods all around the world. In Korea, a guideline for sodium reduction in 27 items and 44 kinds of foods including confectionery was suggested as part of the 'processed food sodium reduction guideline development project', which has been conducted since 2012.

• The monthly packaging world
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• s.283
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• pp.113-117
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• 2016

식품의약품안전처는 의약외품 사용 시 주의해야할 중요 정보를 누구나 이해하기 쉬운 도안 및 도형으로 의약외품의 용기나 포장에 표시하는 방안을 신설하여 소비자의 안전한 의약외품 사용을 도모하고자 의약외품 표시에 관한 규정 일부개정고시를마련했다. 다음에 의약외품 표시에 관한 규정 일부개정고시의 주요 내용에 대해 살펴보도록 한다.

• Korean Journal of Environmental Agriculture
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• v.42 no.2
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• pp.139-151
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• 2023

Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO₄ (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO₄ and C₁₈ (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R²) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

• The monthly packaging world
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• s.280
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• pp.109-113
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• 2016

식품의약품안전처는 의약외품 사용 시 주의해야할 중요 정보를 누구나 이해하기 쉬운 도안 및 도형으로 의약외품의 용기나 포장에 표시하는 방안을 신설하여 소비자의 안전한 의약외품 사용을 도모하고자 의약외품 표시에 관한 규정 일부개정고시안을 행정예고했다. 본 고에서는 주요내용과 품목별 외부 용기나 포장 중 사용상의 주의사항 등 기재요령 및 순서에 대해 살펴보도록 한다.

• Journal of Food Hygiene and Safety
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• v.39 no.3
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• pp.209-220
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• 2024

Cavier is graded as Beluga, Osetra, and Sevruga based on the species of sturgeon (Acipenser sinensis). In this study, we developed an analytical method for determining the grade of black caviar using DNA barcodes and KASP markers. To identify the sturgeon species, ten black caviar samples were collected, and a reference DNA barcode library was developed using five genes (namely, 16S ribosomal RNA, cytochrome b, cytochrome c oxidase subunit I, cytochrome c oxidase subunit II, and NADH dehydrogenase subunit 5 genes). To develop the KASP markers, we selected 11 markers that could distinguish between the five grades of black caviar. As a result, specific markers for each of the targeted caviars were clustered into FAM-positive sections. DNA barcoding and the KASP assay revealed that one Beluga, six Osetra, and three Sevruga were identified among the ten caviar samples. Moreover, we found that the sturgeon species were mislabeled in two products. Here, we aimed to develop a KASP assay based on SNP that allows rapid and easy identification of caviar grade. These methods are expected to contribute to preventing the distribution of illegal products.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.136-142
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• 2022

The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO₄, primary secondary amine (PSA), and octadecyl (C₁₈), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R²) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.