• Analytical Science and Technology
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• v.36 no.2
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• pp.89-98
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• 2023

Analytical methods for detecting atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes were developed using ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). UHPLC-MS/MS conditions were optimized for rapid, sensitive, and simultaneous analysis of the five allergenic compounds. The methods were validated by assessing their specificity, matrix effects, limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and precision. Good linearity was achieved with a determination coefficient of ≥0.99. The LOD and LOQ were 2.1-9.8 and 6.4-29.6 ng/g for sanitary napkins and 0.29-0.48 and 0.87-1.45 ng/mL for mouthwashes, respectively. The accuracy and precision were within an acceptable range according to the criteria reported in the European SANTE/11813/2017 guidelines (70-120 % recovery, <20 % relative standard deviation). Therefore, these methods can be used to analyze atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes.

• KSBB Journal
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• v.30 no.4
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• pp.141-147
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• 2015

The convenient determination of methylsulfonylmethane (MSM) for a commercially available dietary supplement was developed using gas chromatography (GC)-flame ionization detector (FID). Chromatography was performed on a capillary column ($0.32mm\;I.D{\times}30m$, $0.25{\mu}m$) coated with dimethylpolysiloxane using diethylene glycol methyl ether as an internal standard. The performance characteristics of GC were evaluated in terms of selectivity, linearity, precision, accuracy, recovery, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination: 0.9979) within the concentration range of $10.0{\sim}800.0{\mu}g/mL$ for MSM. The recoveries for three fortified concentrations were 96.7~97.1%, 96.6~97.3% and 96.8~97.2%, respectively. The LOD and LOQ of the method were $0.29{\mu}g/mL$ and $0.97{\mu}g/mL$, respectively. All obtained results were acceptable according to the guidelines of the Association of Official Analytical Chemists for dietary supplements. Thus, the validated analytical method using the GC-FID system is suitable for the determination of MSM in dietary supplement formulations for quality control.

• 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.

• Korean Journal of Veterinary Service
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• v.44 no.3
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• pp.125-131
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• 2021

Benzimidazole is an widely used anthelmintics in livestock clinics. The aim of present study was to investigate benzimidazole residues in the meat in Sejong City. A total of 338 samples of meat(beef 287, pork 37, chicken 14) were selected from the laboratory meat(Korean beef genetic test, hygiene test) supplied to school in Sejong City. Representative benzimidazole class drug such as thiabendazole, 2-amino albendazole sulfone, fenbendazole, oxfendazole, and oxfendazole sulfone were monitored in samples by using lc-ms/ms and the analysis was preformed based on the Korea Food Code guideline. Limit of quantitation (LOQ) was ranged from 0.56 to 3.02 ppb for target drugs and the accuracy was within the acceptance criteria. Among the sample analyzed only one case, the pork meat was found to have drug levels that exceed LOQ. However, the overall residue concentration was 2.17 ppb, which was lower than the maximum residue levels (100 ppb).

• 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.

• 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.

• 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.

• Journal of Digital Convergence
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• v.10 no.6
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• pp.331-339
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• 2012

The easy and simple simultaneous analytical method of preservatives (BA, SA, DHA, MP, EP, IPP, PP, IBP and BP) was studied by more easily changing from method used in food and drug using HPLC with scherzo SM-C18 column. All presevatives were seperated successfully in mobile phase of 50 mM ammonium formate : 0.1% phosphoric acid (50:50 v/v%) and 50 mM ammonium formate : acetonitrile (30 : 70). Retention time of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP was 7.74, 9.08, 12.57, 13.83, 21.62, 27.29, 28.20, 33.20 and 33.68 min, respectively. The calibration curves of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP were linear over the concentration range of 5~80 ${\mu}g/mL$ with correlation coefficient of above 0.999. The limit of detection (LOD) and limit of quantitation (LOQ) of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP were 0.52 and 1.58, 1.09 and 3.29, 1.00 and 3.03, 1.36 and 4.13, 1.26 and 3.83, 1.02 and 3.08, 1.11 and 3.37, 0.82 and 2.48, 0.85 and 2.59 ${\mu}g/mL$, respectively. The coefficients of variation for intra- and inter-day assay were 0.12~2.68 and 0.18~2.66%, respectively. The developed method showed good intra- and inter-day precision and accuracy. The preservatives used in mouthwashes were BA, MP and PP and were detected in 24 samples(86%) except for 4 samples and not showed significant difference in using dose of adult and children. In conclusion, the developed method can be useful for simultaneous analysis of preservatives in mouthwashes and these results suggest that could be applied to fundamental study and guideline on content of preservatives in mouthwashes.