• Journal of Food Hygiene and Safety
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• v.35 no.5
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• pp.411-418
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• 2020

In this study, we reviewed a group of marine biotoxins, namely yessotoxins (YTXs), focusing on their causative organisms, contaminated shellfish, domestic and foreign management status, and analytical methods. Although YTXs have not yet been reported in any cases of seafood contamination in South Korea, it is necessary to implement preemptive measures through continuous monitoring because there is a potential risk, due to the introduction of toxic microalgae associated with climate changes and the introduction of contaminated seafood from various countries. YTXs are produced by dinoflagellates, such as Protecratium reticulatum, Gonyaulax polygramma, Gonyaulax spinifera, and Lingulodinium polyedrum, all of which are species found along Korea's coastal areas. Analysis of YTXs in shellfish samples is mainly performed by use of LC-MS/MS after methanol extraction and SPE cartridge clean-up (HLB or strata-X). In the case of lipophilic marine biotoxins, including YTXs, pectenotoxins, and azaspiracids, the extraction and purification procedures are similar. Thus, it seems that the simultaneous analysis of several lipophilic marine biotoxins in shellfish samples is possible, and optimization is necessary. In addition, continuous monitoring studies on causative marine microalgae for YTXs in Korean coastal waters and contaminations in domestic and imported seafood are needed.

• Korean Journal of Food Science and Technology
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• v.37 no.2
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• pp.304-307
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• 2005

Multiresidue method was set up for the simultaneous determination of various residual pesticides in potatoes and carrots, which was analyzed by gas chromatography-electron capture detector/nitrogen phosphorus detector. Method consisted with acetone/acetonitrile (9 : 1) extraction and dichloromethane partition, followed by florisil cartridge purification with hexane/dichloromethane/acetonitrile (50 : 45 ; 5) elution. Among 197 pesticides (194 kinds) spiked to food materials, 143 and 155 pesticides were recovered over 70% on potatoes and carrots, respectively. Nineteen pesticides including bromacil, cyproconazole, were not detected in water and sample matrices. Matrix components may affect the low detections of 25 pesticides such as benfuracarb, bitertanol from potatoes and 16 pesticides such as bitertanol, carbosulfan from Carrots. Some pesticides including dichlobenil, fluoroimide and iprodione were highly detected from one or both matrices even though they were not detected from water.

• Korean Journal of Soil Science and Fertilizer
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• v.31 no.1
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• pp.67-71
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• 1998

This study was carried out to granulate artificial zeolite powder that remove ammonium nitrogen and phosphorous simultaneously in wastewater treatment. Optimum water content was required for 30 percent volume to granulate artificial zeolite with 1.7mm diameter and 1~2cm length using granulator. Portland cement could remove much $NH_4{^+}$ and $PO_4{^{3-}}$ from the wastewater than other binding materials. Mixed 33, 25. 20. 16 percent of portland cement to artificial zeolite powder(v/v), cation exchange capacity of the granulars were 66.5, 81.4, 126.8, $151.2cmol^+kg^{-1}$ and hardness of that were 176.1, 24.4, 4.1, $0.4kg\;cm^{-2}$, respectively. Content of portland cement in the granular were related with removal of $PO_4{^{3-}}$ positively and that of $NH_4{^+}$ negatively. Shaked 1g of the granulars that made of portland cement 33 percent with 40ml synthetic wastewater containing $NH_4{^+}$ $1545mgl^{-1}$ and $PO_4{^{3-}}$ $417mgl^{-1}$, 99.4 percent of $NH_4{^+}$ and 90.3 percent of $PO_4{^{3-}}$ were removed simultaneously after 48 hours shaking. The longer shaking, the more $NH_4{^+}$ and $PO_4{^{3-}}$were removed. The artificial zeolite granular had both micropore and macropore that could be useful in the wastewater purification.

• Journal of Environmental Impact Assessment
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• v.29 no.6
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• pp.403-413
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• 2020

A mathematical model comprised with eight simultaneous quasi-linear partial differential equations was suggested to provide optimal chlorination strategy. Upstream weighted finite element method was employed to construct multidimensional numerical code. The code was verified against measured concentrations in three type of reactors. Boundary conditions and reaction rate were calibrated for the sixteen cases of experimental results to regenerate the measured values. Eight reaction rate coefficients were estimated from the modeling result. The reaction rate coefficients were expressed in terms of pH and temperature. Automatic optimal algorithm was invented to estimate the reaction rate coefficients by minimizing the sum of squares of the numerical errors and combined with the model. In order to minimize the concentration of chlorine and pollutants at the final usage sites, a real-time predictive control system is imperative which can predict the water quality variables from the chlorine disinfection process at the water purification plant to the customer by means of a model and operate the disinfection process according to the influent water quality. This model can be used to build such a system in water treatment plants.

• Food Science and Industry
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• v.55 no.1
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• pp.58-73
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• 2022

Due to the recent demand for low-calorie foods, consumers are looking for alternative sweeteners that can control blood sugar, low risk of tooth decay and low calories. Regulations for permitted sweeteners in food vary from every country, and it is important for the government and the food industry to monitor products containing these sweeteners to ensure global compliance. Therefore, rapid, precise, and accurate analysis for food matrices should be applied to quality control, market surveillance, monitoring, and evaluation of food additive intake in the food industry. To analyze sweeteners simultaneously, it is essential to develop an efficient and rapid analytical method and to perform appropriate pretreatment steps such as solvent extraction and purification. This study presented the recent analysis trends about the suitable extraction method for food matrices focusing on non-nutritive sweeteners. Additionally, techniques for multi-compounds analysis using HPLC and LC-MS/MS and non-destructive analysis techniques using FT-IR were comprehensively described.

• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.201-210
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• 2017

BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

• Analytical Science and Technology
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• v.31 no.4
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• pp.161-170
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• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Journal of Food Hygiene and Safety
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• v.31 no.2
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• pp.85-93
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• 2016

A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

• Journal of Food Hygiene and Safety
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• v.33 no.3
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• pp.176-184
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• 2018

The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.158-169
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• 2019

Ergot alkaloids are mycotoxin produced by fungi of the Claviceps genus, mainly by Claviceps purpurea in EU. Recently obtained informations indicates necessity for control the ergot in imported grains. Recent occurrence data of ergot alkaloids from EU countries indicate the necessities of management and control these toxins from the imported grains like rye, wheat, oat etc. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine and their epimers (-inines) from grain and grain-based food. The test method was optimized by extracting the sample with acetonitrile containing 2 mM ammonium carbonate, purification with Mycosep cartridge, and instrumental analysis by LC-MS/MS using Syncronis C18 column. The standard calibration curves showed linearity with correlation coefficents; $R^2$ >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and $100{\mu}g/kg$). The correlation coefficient expressed as precision was within the range of 1.9-12.9%. The limit or quantifications (LOQ) ranged from 0.012 to $0.058{\mu}g/kg$. The developed analytical method met the criteria of AOAC Int. and CAC validation parameters like accuracy and sensitivity. As a result, it was confirmed that the test method developed in this study is suitable for the simultaneous analysis of six species of ergot alkaloid from grains and grain products.