• Journal of Food Hygiene and Safety
• /
• v.33 no.2
• /
• pp.110-117
• /
• 2018

The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

• Korean Journal of Environmental Agriculture
• /
• v.42 no.1
• /
• pp.71-81
• /
• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Journal of Environmental Health Sciences
• /
• v.22 no.1
• /
• pp.45-50
• /
• 1996

The application of HACCP system, which was adopted by Codex Alimentarius Committee for the safe meat and poultry production, is one of the urgent task for competing in the world trade markets. But there have been no useful analytical studies to identify the causes of contamination in the poultry meat processing plants in Korea. This study was conducted to investigate the potential hazards during the operations by the microbiological examination for the poultry meat processing plant (20,000 birds capacity a day) located in Kangwon province. In spite of air contamination of work places, it may not directly affect the surface contamination of poultry meats. But the risk of Campylobacter jejuni/coli contamination was high. The number of total count was decreased about ten times, but remarkable changes of microbial contamination could not be recognized in each procedure during the operations. The washing water was already contaminated as much as $10^{3-6}CFU/ml$ in SPC before the operations. It means that to keep water tanks hygienic is a primary step to prevent the occurrences of microbial contamination. The overflow and recirculation of water in scalding, washing, and chilling was aslo an important factor for a hygienic control. Based on this study, the followings could be regarded as an important factors for hygenic control in the poultry slaughtering plants on a small scale. The temperature of water used for scalding should be constantly maintained on a required temperature, and the overflow rate of 1~1.5 liter per bird. The carcass surface and the body cavity should be washed thoroughly and the cross-contamination due to facilities, workers, and tools should be prevented. The chilling water sholud be maintained under 5$\circ$C of temperature with ice and overflow, and residual chlorine level of 50 ppm.

• Korean Journal of Organic Agriculture
• /
• v.8 no.1
• /
• pp.111-129
• /
• 1999

In order to get some basic data to check the environmental sound function against soil and water pollution and the safe vegetable production by korean organic farming where an internationally recognized basic concepts of soil fertility management for organic farming is not practiced and only applying the organic fertilizer to maintain the soil fertility, the chemical characteristics of soils and $NO_{3}^{-}$ content of chinese cabbage and lettuce cultivated by the conventional farming, greenhouse cultivation and organic farming were investigated. The highest value of $NO_{3}^{-}$-N in 0~30cm subsoil among the three different farming systems was found in the subsoil of organic farming and it was 3.6 and 6.6 times higher than those of conventional farming in chinese cabbage and lettuce respectively. $P_2O_5$ accumulation in the rhizosphere by organic farming also showed the highest value. The accumulation of $NO_{3}^{-}$-N and $P_2O_5$ in organic farming soil were similar or even more higher to those of greenhouse cultivation. The $NO_{3}^{-}$ accumulation in the vegetable by organic farming reached 3224ppm for chinese cabbage and 2543ppm for lettuce, and it were 4.7 and 6.4 times higher than those by conventional farming. It was concluded that there is urgently necessary to introduce the main concepts of soil fertility management of the Basic Standard of IFOAM, EU regulation and FAO/WHO Codex Alimentarius on organic agriculture(draft) into korean organic agriculture for the operation of environmental sound system and the production of sate vegetable in terms of $NO_{3}^{-}$ content.

• The Korean Journal of Pesticide Science
• /
• v.4 no.4
• /
• pp.1-11
• /
• 2000

Since the chemical pesticides have been played a major role in crop protection practices during last 5 to 7 decades, social concerns on the pesticide residues in and on food commodities as well as environmental compartments have also growing with endless demands and interests. Most national regulation authorities over the world have paid a special attention on the data requirements for pesticide registration. In addition, even the registered pesticides also should follow the re-registration process, which meets today's guidelines and regulatory triggers and safety profiles. More recently, a defined interest in the international bodies has given to the global conservation program from the environmental contamination; these involves persistent organic pollutants (POPs), endocrine disrupting chemicals (EDs), biocides, etc.. In order to secure the food safety and keep our circumference sound, in-depth efforts getting information from global networks have perpetually to be given under relevant national agencies. At the same time, a nation-wide survey of the residues has also to be in operation to monitor the tendency of the toxicant in/on foods, feeds, and environmental segments. In final, the scientifically assessed results on safety should be opened to the public to provide the right-to-know for the consumers.

• Nutrition Research and Practice
• /
• v.1 no.2
• /
• pp.89-93
• /
• 2007

Many countries such as The Republic of Korea have established their own nutritional standards, collectively termed Nutrient Reference Values (NRVs), and they vary due to the science which was reviewed, the purposes for which they are developed, and issues related to nutrition and food policy in the country. The current effort by the Codex Alimentarius Committee on Nutrition and Foods for Special Dietary Uses (CNFSDU) to update the NRVs that were established following the Helsinki Consultation in 1988 represents an opportunity to develop a set of reference values reflecting current scientific information to be used or adapted by many countries. This paper will focus on possible approaches to selecting or developing reference values which would serve the intended purpose for nutrition labeling to the greatest extent possible. Within the United States, the Food and Drug Administration (U.S. FDA) is currently reviewing regulations on nutrition labeling to better address current health issues, and is expected to enter into a process in the next few months to begin to explore how best to update nutrient Daily Values (DVs), most of which are still based on the Recommended Dietary Allowances (RDAs) of the Food and Nutrition Board, U.S. National Academy of Sciences, last reviewed and revised in 1968. In this presentation, I review the current purposes in the U.S. for nutrition labeling as identified in the 1938 Food, Drug, and Cosmetic Act as amended, the scientific basis for current nutrition labeling regulations in the United States, and the recommendations made by the recent Committee on Use of Dietary Reference Intakes in Nutrition Labeling of the Institute of Medicine (2003) regarding how to use the DRIs in developing new DVs to be used on the label in the United States and Canada. Based on these reviews, I then provide examples of the issues that arise in comparing one approach to another. Much of the discussion focuses on the appropriate role of nutrient labeling within the Nutrition Facts panel, one of the three major public nutrition education tools in the United States (along with MyPyramid and Dietary Guidelines for Americans).

• Korean Journal of Environmental Agriculture
• /
• v.39 no.4
• /
• pp.368-374
• /
• 2020

BACKGROUND: The residual analysis of polar pesticides has remained a challenge. It is even more difficult to simultaneously analyze multiple polar pesticides. Diquat, paraquat, and chlormequat are typical examples of highly polar pesticides. The existing methods for the analysis of diquat, paraquat and chlormequat are complex and time consuming. Therefore, a simple, quick and effective method was developed in the represent study for simultaneous analysis of diquat, paraquat and chlormequat in animal products, meat and fat using UPLC-MS/MS. METHODS AND RESULTS: Sample extraction was carried out using acidified acetonitrile and water and re- extracted with acidified acetonitrile and combine the extracts followed by centrifugation. The extract was then cleaned up with a HLB cartridge after reconstitution with acidic acetonitrile and water. The method was validated in quintuplicate at three different concentrations. The limits of detection (LOD) and quantification (LOQ) were 0.0015 and 0.005 mg/L, respectively. Matrix suppression effect was observed for all of the analytes. A seven point matrix matched calibration curve was constructed for each of the compound resulted excellent linearity with determination coefficients (R2) ≥ 0.991. Accuracy and precision of the method was calculated from the recovery and repeatability and ranged from 62.4 to 119.7% with relative standard deviation less than 18.8%. CONCLUSION: The recovery and repeatability of the developed method were in the acceptable range according to the Codex Alimentarius guideline. The developed method can be applied for the routine monitoring of diquat, paraquat, and chlormequat in animal products, meat and fat.

• Analytical Science and Technology
• /
• v.34 no.1
• /
• pp.1-8
• /
• 2021

An analytical method was developed and optimized for the quantification of a plant growth regulator, 2,6-diisopropylnaphthalene (2,6-DIPN), in agricultural products using gas chromatography-tandem mass spectrometry. The samples were extracted, partitioned, and were purified using a Florisil® cartridge. To validate the analytical method, its specificity, linearity, limit of detection (LOD) and limit of quantification (LOQ) of the instrument, LOQ of the analytical method (MLOQ), accuracy, and repeatability were considered. The method displayed excellent results during validation, and is suitable for the determination and quantification of the low residual levels of the analyte in the agricultural samples. All of the results with the optimized method were satisfactory and within the criteria ranges requested in the Codex Alimentarius Commission guidelines and the Ministry of Food and Drug Safety guidelines for pesticide residue analysis. The developed method is simple and accurate and can be used as a basis for safety management of 2,6-DIPN.

• Korean Journal of Environmental Agriculture
• /
• v.37 no.4
• /
• pp.283-290
• /
• 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
• /
• v.34 no.1
• /
• pp.30-39
• /
• 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.