• 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.

• Journal of Food Hygiene and Safety
• /
• v.34 no.3
• /
• pp.242-250
• /
• 2019

An analytical method was developed for the determination of fenquinotrione, a triketone herbicide, in agricultural products. Fenquinotrione was metabolized to KIH-3653-M-2 in plants. Analyte extraction was conducted using 2% formic acid in acetonitrile and cleaned up using a hydrophillic-lipophillic balance (HLB) cartridge. The limits of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. Matrix-matched calibration curves were linear over the calibration ranges ($0.001{\sim}0.1{\mu}g/mL$) into a blank extract with $r^2>0.99$. The recovery results for fenquinotrione and KIH-3653-M-2 ranged between 81.1 to 116.2% and 78.0 to 110.0% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$) with relative standard deviation (RSD) less than 4.6%. All values were corresponded with the criteria ranges requested in both the Codex (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of fenquinotrione in the Republic of Korea.

• Journal of Food Hygiene and Safety
• /
• v.36 no.3
• /
• pp.220-227
• /
• 2021

Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO₄ and NaCl were used with acetonitrile. C₁₈ (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

• Journal of Food Hygiene and Safety
• /
• v.36 no.3
• /
• pp.248-256
• /
• 2021

A total of 120 samples corresponding to 12 categories of dried processed fishery products distributed in Gyeonggi-do were examined for radioactivity contamination (¹³¹I, ¹³⁴Cs, ¹³⁷Cs) and heavy metals (lead, cadmium, arsenic, and mercury). One natural radioactive material, ⁴⁰K, was detected in all products, while the artificial radioactive materials ¹³¹I, ¹³⁴Cs and ¹³⁷Cs were not detected at above MDA (minimum detectable activity) values. The detection ranges of heavy metals converted by biological basis were found as follows: Pb (N.D.-0.332 mg/kg), Cd (N.D.-2.941 mg/kg), As (0.371-15.007 mg/kg), Hg (0.0005-0.0621 mg/kg). Heavy metals were detected within standard levels when there was an acceptable standard, but the arsenic content was high in most products, although none of the products had a permitted level of arsenic. In the case of dried processed fishery products, there are products that are consumed by restoring moisture to its original state, but there are also many products that are consumed directly in the dry state, so it will be necessary to set permitted levels for heavy metals considering this situation in the future. In addition, Japan has decided to release contaminated water from the Fukushima nuclear power plant into the ocean, so there is high public concern about radioactivity contamination of food, including fishery products. Therefore, continuous monitoring of various food items will be necessary to ease consumers' anxiety.

• Korean Chemical Engineering Research
• /
• v.60 no.4
• /
• pp.594-605
• /
• 2022

CaO was prepared by calcining for oyster shells using a microwave kiln. It was analyzed to Ca(OH)₂ synthed on hydration reaction from prepared CaO. The synthesized Ca(OH)₂ was formulated as an external water paint. Oyster shells (325 mesh, 43 ㎛) were decarbonized for (a) 950 ℃/1 hr and (b) 1,150 ℃/1 hr to prepare CaO. In the calcination condition of (a), CaO was 56.7 wt%, and in the calcination condition of (b), CaO was 100 wt%. To compare CaO by calcination of oyster shells with that of limestone, limestone (25~30 mm) was decarbonized at 950 ℃/1 hr to prepare CaO, and as a result of the analysis(XRD), it was analyzed as CaO 100 wt%. CaO was prepared under the calcining conditions of oyster shells (b) 1,150 ℃/1 hr, and Ca(OH)₂ was synthesized through hydration. Hydration conditions of the prepared CaO were (a) CaO : H₂O(100 g : 200 g) and (b) CaO : H₂O(100 g : 400 g). As a result of the hydration reaction, it was confirmed as low reactivity. 100 wt% of Ca(OH)₂ was synthesized. In particular, Ca(OH)₂ synthesized under the hydration condition of (a) was analyzed in a plate shape. An external water paint was formulated with Ca(OH)₂ synthesized from oyster shells as the main component. When 15 items of the external water paint standard specification (KS M 6010) were analyzed, it was confirmed that all other criteria were satisfied except for freezing stability.

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