• Analytical Science and Technology
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• v.25 no.5
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• pp.307-312
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• 2012

To perform inhalation toxicity test by using experiment animals, we set up an analytical method to monitor didecyldimethylammonium chloride (DDAC) in aerosol nebulized into inhalation chambers by ion chromatography. DDAC was adsorbed by XAD-2 resin and analyzed with conductivity detector. Recovery of DDAC desorbed by acetonitrile from XAD adsorbent was 87.8%. The method detection limit (MDL) and the limit of quantitation (LOQ) were 2.97 ${\mu}g/m^3$ and 8.92 ${\mu}g/m^3$, respectively. Repeatability was calculated as RSD 7.8% in the range of 0~20 ${\mu}g/mL$. Time needed to analyze a sample was less than 5 minutes. Therefore, the analysis of DDAC by ion chromatography was practically useful in monitoring DDAC in inhalation chambers with rapidity and sensitivity manner to perform inhalation toxicity test using experimental animals.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.130-137
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• 2020

BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r²>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by 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 mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

• Journal of Digital Convergence
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• v.10 no.7
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• pp.201-206
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• 2012

Benzo(a)pyrene is a polycyclic aromatic hydrocarbons (PAHs) whose metabolites are mutagenic and highly carcinogenic and is listed as a Group 1 carcinogen by the IARC. It has been found at variable concentrations in several foods and is associated with several factors during the process including contaminated raw materials, exposure of environment, and procedure of process or cooking. In this study, benzo(a)pyrene in 45 oriental medicines were determined by HPLC/FLD. The calibration curves of benzo(a)pyrene was linear over the concentration range of 0.5~40 ng/mL with correlation coefficient of above 0.999. The limit of detection (LOD) and limit of quantitation (LOQ) of benzo(a)pyrene were 0.04 and 0.10 ${\mu}g/kg$. Benzo(a)pyrene in 3 samples out of 45 samples was not detected. The level of benzo(a)pyrene in 26 (57.7%), 8 (17.8%) and 7 (15.6%) samples was 0.1~0.5, 0.5~1.0 and 1.0~5.0 ${\mu}g/kg$, respectively. Especially, content of benzo(a)pyrene in Coptis Rhizome is the highest (5.97 ${\mu}g/kg$). In conclusion, these results suggest that could be applied to fundamental study and guideline on drying condition to decrease content of benzo(a)pyrene in oriental medicine.

• Journal of Korean Society of Environmental Engineers
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• v.36 no.6
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• pp.387-395
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• 2014

A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC-MS/MS) has been developed, allowing the simultaneous multi-analyte determination of 11 synthetic fragrances (SFs) in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 10.9%). The extraction efficiencies were above 83% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~4.1 ng/L and 6.6~12.9 ng/L, respectively. The developed method offers the ability to detect 11 SFs at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 11 SFs. The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.

• Korean Journal of Food Science and Technology
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• v.51 no.5
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• pp.420-424
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• 2019

An HPLC analysis method was developed and standardized for the detection of dieckol as a functional food ingredient in Ecklonia cava extracts. HPLC was performed using a Capcell Pak C18 column ($250{\times}4.6mm$, $5{\mu}m$) with a gradient elution of water and acetonitrile, both containing 0.1% (v/v) trifluoroacetic acid, at a flow rate of 1.0 mL/min at $25^{\circ}C$. The eluate was detected at 230 nm. For validation, the specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) of dieckol were measured. The calibration curve for the detection of dieckol had high linearity ($R^2=0.9994$), with LOD and LOQ values of 0.38 and $1.16{\mu}g/mL$, respectively. Recovery of the quantified compound ranged from 99.61 to 100.71%. The relative standard deviation values of the intra-day and inter-day precisions were less than 1.7 and 1.25%, respectively. These results indicate that the reported HPLC method is simple, reliable, and reproducible for the detection of dieckol in Ecklonia cava extracts.

• Food Engineering Progress
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• v.15 no.1
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• pp.75-79
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• 2011

Analytical methods for food antioxidants including ascorbic acid, erythorbic acid, ascorbyl palmitate (AP), and ascorbyl stearate (AS), were validated using high performance liquid chromatography. Validation parameters such as linearity, limit of detection (LOD), limit of quantification (LOQ), and recovery were tested using lard and cider as food model systems. Linearity of ascorbic acid and erythorbic acid were both higher than ($R^2$> 0.99), LOD of these compounds were 0.46 and 0.48 ${\mu}g/mL$, respectively and LOQ were 1.39 and 1.45 ${\mu}g/mL$, respectively. The recovery rates of these compounds were 86.35-94.78% and 84.76-95.02%, respectively. However, the concentration of AP and AS decreased in methanol stock solution. Four other solvents including ethanol, acetonitrile, mixture of methanol and acetonitrile, and mixture of ethanol and acetonitrile were tested to increase the stability of AP and AS under room temperature and refrigerated temperature. Ethanol provided better stability of AP and AS under both room and refrigerated temperature. This study can help to accurately analyze the content of ascorbic acid and its derivatives in processed foods.

• Journal of Food Hygiene and Safety
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• v.36 no.1
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• pp.34-41
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• 2021

The purpose of this research is to improve analysis methods of determining the contents of fatty acids in infant formulas and follow-up formulas. A gas chromatography (GC) method was performed on a GC system coupled to flame ionization detector, with a fused silica capillary column (SP2560, 100 m×0.25 mm, 0.20 ㎛). The method was validated using standard reference material (SRM, NIST 1849a). Performance parameters for method validation such as specificity, linearity, limits of detection (LOD) and quantification (LOQ), accuracy and precision were examined. The linearity of standard solution with correlation coefficient was higher than 0.999 in the range of 0.1-5 mg/mL. The LOD and LOQ were 0.01-0.06 mg/mL and 0.03-0.2 mg/mL, respectively. The recovery using standard reference material was confirmed and the precision was found to be between 0.8% and 2.9% relative standard deviation (RSD). Optimized methods were applied in sample analysis to verify the reliability. All the tested products had acceptable contents of fatty acids compared with component specification for nutrition labeling. The result of this research will provide efficient experimental information and strengthen the management of nutrients in infant formula and follow-up formula.

• Fisheries and Aquatic Sciences
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• v.25 no.12
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• pp.626-636
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• 2022

Shellfish are exoskeleton-bearing aquatic invertebrates that consume various organic and inorganic substances floating in seawater through filter feeding. Heavy metals are known as absorbed and accumulated in seawater. Some of the toxic heavy metals are highly accumulated in seawater, and exposure to them can cause a variety of risks to the human body. Since Koreans like to eat seafood, they are more likely to be exposed to contaminated seafood with heavy metals. In this study, nine types of heavy metals were analyzed on ten different shellfish species in the coastal area of South Korea. The risk assessment was also done on shellfish in which heavy metals were detected. Zinc (Zn) and copper (Cu) were identified at an average of 56.7 mg/kg (6.70 to 466 mg/kg) and 13.2 mg/kg (0.064 to 143 mg/kg), respectively. Lead (Pb) average of 0.208 mg/kg (0.000750 to 1.02 mg/kg), cadmium (Cd) average of 0.454 mg/kg (0.0388 to 1.56 mg/kg) and mercury (Hg) average of 0.0266 mg/kg (0.00548 to 0.174 mg/kg) were identified. Additionally, arsenic (As), chromium (Cr), nickel (Ni), and silver (Ag) were also identified as average concentrations of 4.02 (0.460 to 15.0 mg/kg), 0.167 (< limit of quantification [LOQ] to 0.820 mg/kg), 0.281 (< LOQ to 1.46 mg/kg), and 0.158 mg/kg (< LOQ to 1.15 mg/kg). The result indicates that the monitoring results of heavy metals in most shellfish satisfied the Korean standard. However, Pb and Cd have exceeded some foreign standards, such as the United States and the EU. The permissible human exposure calculated using the heavy metal intake and detection amount was lower than the Joint FAO/WHO Expert Committee on Food Additives human safety standard, and the risk of heavy metals from shellfish consumption was at an acceptable level.

• 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.

• Analytical Science and Technology
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• v.19 no.5
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• pp.441-448
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• 2006

11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH) is the major metabolite of tetrahydrocannabinol (THC) which is the primary psychoactive component of marijuana. It is also the target analyte for the discrimination marijuana use. A method using solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of THCCOOH in human urine. Urine samples (3 mL) were extracted by SPE column with a cation exchange cartridge after basic hydrolysis. The eluents were then evaporated, derivatized, and injected into the GC/MS. The limits of detection (LOD) and quantitation (LOQ) were 0.4 and 1.2 ng/mL, respectively. The response was linear with a correlation coefficient of 0.999 within the concentration range of 1.2 (LLE 1.3)~50.0 ng/mL. The precision and accuracy were stable within 1.20% and the recovery was 83.6~90.7%. The recovery of SPE method was lower than that of liquid-liquid extraction (LLE), but there were no apparent differences in LOD, LOQ, precision and accuracy between the two methods. While SPE method is used as a very effective and rapid procedure for sample pretreatment, and clean extracts, LLE method was not suitable for the extraction procedure of THCCOOH in urine. The applicability of the method was proven by analyzing a urine samples from a marijuana abusers.