• 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.3
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• pp.283-289
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• 2019

This study was performed to monitor the residual pesticides in agricultural products used in school foodservice in the Gwangju metropolitan area. Risk assessment was also carried out based on the amount of agricultural products consumed. A total of 320 agricultural products supplied to schools in Gwangju were analyzed from 2015 to 2017. The pre-treatment and residual pesticide analysis of these products was conducted in accordance with the second method for multi-residue analysis of pesticides in the Korean food code. The hazard index was calculated by dividing the estimated daily intake (EDI) of pesticides by the acceptable daily intake (ADI). The linearity correlation coefficient for the calibration curve was 0.9923 to 1.0000, LOD 0.004 to 0.019 mg/kg, LOQ 0.012 to 0.057 mg/kg, and recovery was 79.1 to 100.2%. Residual pesticides were detected in 18 (5.6%) of 320 agricultural products used for school foodservice, and one sample of sweet potato stem (0.3%) exceeded the maximum residual limit (MRL). The detection frequency for chili peppers and bell peppers was higher than that for other agricultural products. The frequently-detected pesticides were boscalid and acetamiprid. These results showed that residual pesticide management is needed for chili pepper, bell pepper and sweet potato stem among agricultural products supplied to schools. The hazard index of bifenthrin in sweet potato stem showed the highest (64.18%), and the other pesticides were 0.03-8.23%. These results indicated that agricultural products supplied to schools in Gwangju were safe for consumption. To minimize the intake of residual pesticides, it is necessary to not only thoroughly wash agricultural products but to also ensure the expanded supply of products that are pesticide-free.

• 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.

• Journal of Food Hygiene and Safety
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• v.36 no.1
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• pp.24-33
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• 2021

For this study, we surveyed concentrations of 8 mycotoxins (aflatoxin B1, B2, G1, G2, ochratoxin A, fumonisin B1, B2 and zearalenone) in agricultural products used for food and medicine by liquid chromatography-tandem mass spectrometry and conducted a risk assessment. Samples were collected at the Yangnyeong Market in Seoul, Korea, between January and November 2019. Mycotoxins were extracted from these samples by adding 0.1% formic acid in 50% acetonitrile and cleaned up by using an ISOLUTE Myco cartridge. The method was validated by assessing its matrix effects, linearity, limit of detection (LOD), limit of quantification (LOQ), recovery and precision using four representative matrices. Matrix-matched standard calibration was used for quantification and the calibration curves of all analytes showed good linearity (r2>0.9999). LODs and LOQs were in the range of 0.02-0.11 ㎍/kg and 0.06-0.26 ㎍/kg, respectively. Sample recoveries were from 81.2 to 118.7% and relative standard deviations lower than 8.90%. The method developed in this study was applied to analyze a total of 187 samples, and aflatoxin B1 was detected at the range of 1.18-7.29 ㎍/kg (below the maximum allowable limit set by the Ministry of Food and Drug Safety, MFDS), whereas aflatoxin B2, G1 and G2 were not detected. Mycotoxins that are not regulated presently in Korea were also detected: fumonisin (0.84-14.25 ㎍/kg), ochratoxin A (0.76-17.42 ㎍/kg), and zearalenone (1.73-15.96 ㎍/kg). Risk assessment was evaluated by using estimated daily intake (EDI) and specific guideline values. These results indicate that the overall exposure level of Koreans to mycotoxins due to the intake of agricultural products used for food and medicine is unlikely to be a major risk factor for their health.

• Korean Journal of Food Science and Technology
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• v.52 no.6
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• pp.565-572
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• 2020

The 3-monochloropropane-1,2-diol (3-MCPD) is a contaminant that occurs in foodstuffs in its free form as well as in its bound form. The objective of this study was to evaluate the effects of emulsifier, frying temperature, and the amounts of salt and oil on the formation of bound 3-MCPD in a fried snack model. Emulsifier affected the formation of bound 3-MCPD; furthermore, it was observed that the largest amount of bound 3-MCPD was detected in the fried snack model when glycerin esters of fatty acids were used as emulsifiers. Frying temperature also affected the formation of bound 3-MCPD, which increased significantly as the frying temperature increased from 145 to 190℃. In addition, salt affected the formation of bound 3-MCPD. As the amount of salt increased, the amount of bound 3-MCPD also increased significantly. Moreover, it was observed that the amount of oil did not affect the formation of bound 3-MCPD. These results will aid in the reduction of bound 3-MCPD in fried snacks.

• Journal of Food Hygiene and Safety
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• v.35 no.6
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• pp.544-551
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• 2020

The aim of this study was to develop and validate a simultaneous analytical method for berberine and palmatine, which are representative substances of Phellodendron amurense, and to evaluate the antioxidant activity. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for berberine and palmatine using high-performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for berberine and palmatine exhibited 0.9999. The LODs for berberine and palmatine were 0.32 to 0.35 µg/mL and the LOQs were 0.97 to 1.06 µg/mL, respectively. The inter-day and intra-day precision values for berberine and palmatine were from 0.12 to 1.93 and 0.19 to 2.89%, respectively. The inter-day and intra-day accuracies were 98.43-101.45% and 92.39-100.60%, respectively. In addition, the simultaneous analytical method was validated for the detection of berberine and palmatine. Moreover, we conducted FRAP and NaNO2 scavenging activity assays to measure the antioxidant activities of berberine and palmatine, and both showed antioxidant activity. These results suggest that P.amurense could be a potential natural resource for antioxidant activity and that the efficacy can be confirmed by investigating the content of the berberine and palmatine.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.143-148
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• 2022

This study was to investigate an analytical method for determining dieckol content in Ecklonia stolonifera extract. According to the guidelines of International Conference on Harmonization. Method validation was performed by measuring the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of dieckol using high-performance liquid chromatography-photodiode array. The results showed that the correlation coefficient of calibration curve (R²) for dieckol was 0.9997. The LOD and LOQ for dieckol were 0.18 and 0.56 ㎍/mL, respectively. The intra- and inter-day precision values of dieckol were approximately 1.58-4.39% and 1.37-4.64%, respectively. Moreover, intra- and inter-day accuracies of dieckol were approximately 96.91-102.33% and 98.41-105.71%, respectively. Thus, we successfully validated the analytical method for estimating dieckol content in E. stolonifera extract.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.216-224
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• 2022

This study was aimed at validating the analysis methods for deacetylasperulosidic acid (DAA), total sugar, galacturonic acid, glucose, and galactose, which are the indicator components of fermented Morinda citrifolia polysaccharide extract (Vitalbos). We modified the previously reported methods for validating the analytical methods. The specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) were measured using phenol-sulfuric acid method and high-performance liquid chromatography (HPLC). The retention time and spectrum of the standard solution of Vitalbos coincided, confirming the specificity. The calibration curve correlation coefficient (R²), of five indicator components, ranged from 0.9995-0.9998, indicating excellent linearity of 0.99 or more. The intra-day and inter-day precision range of the assay was 0.14-3.01%, indicating a precision of less than 5%. The recovery rate was in the range of 95.13-105.59%, presenting excellent accuracy. The LOD ranged from 0.39 to 0.84 ㎍/mL and the LOQ ranged from 1.18 to 2.55 ㎍/mL. Therefore, the analytical method was validated for DAA, total sugar, galacturonic acid, glucose, and galactose, in Vitalbos. The indicator component content in Vitalbos was determined using a validated method. The contents of DAA, total sugar, galacturonic acid, glucose, and galactose were 2.31±0.06, 475.92±5.95, 72.83±1.05, 71.63±2.44, and 67.30±2.31 mg/g of dry weight, respectively. These results suggest that the developed analytical method is efficient and could contribute to the quality control of Vitalbos, as a healthy functional food material.

• 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.

• Journal of Applied Biological Chemistry
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• v.63 no.2
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• pp.153-159
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• 2020

The analytical method was established for simultaneous determination of fungicide prochloraz and its metabolites in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). Samples including beef meat, pork meat, chicken meat, milk, and egg were hydrolyzed with pyridine hydrochloride which converts prochloraz and its metabolites to 2,4,6-trichlorophenol (2,4,6-TCP) because residue definition for prochloraz was 'sum of prochloraz and its metabolites containing the 2,4,6-trichlorophenol moiety, expressed as prochloraz', for compliance with MRLs from animal commodities. Therefore, residual prochloraz was extracted with acetone, decomposed to 2,4,6-TCP, partitioned with dichloromethane, purified with aminopropyl SPE and quantified as 2,4,6-TCP with GC-ECD. The instrumental limit of quantitation and method LOQ (MLOQ) was 0.01 ㎍/mL and 0.02 mg/kg for prochloraz and 0.005 ㎍/mL and 0.01 mg/kg for 2,4,6-TCP, respectively. The linearity of the calibration curve was good with R² >0.995 in the range of 0.005-0.2 ㎍/mL. Fortification levels of prochloraz were 0.02 mg/kg (MLOQ) and 0.2 mg/kg (10MLOQ) for recovery tests. Overall recoveries of prochloraz were >90% with <10% of coefficient variation (C.V.). This established analytical method was fully validated and could be useful for quantification of prochloraz and its metabolites in animal commodities as official analytical method.