• Analytical Science and Technology
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• v.25 no.1
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• pp.39-49
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• 2012

A method to detect 37 volatile organic compounds (VOCs) in surface water was described based on headspace solid-phase micro extraction and gas chromatography-mass spectrometry. VOCs in water were vaporized for 30 min at 40 $^{\circ}C$ in a headspace vial and adsorbed on 85 ${\mu}m$ carboxen-polydimethylsiloxane. Under the established condition, the lowest quantification limit was 4.1-96 ng/L by using 4.0 mL water sample, and the relative standard deviation was less than 15% at concentrations of 0.05 and 0.50 ${\mu}g/L$. The detection limits meet lower concentration than 1/10 of the water quality criteria for VOCs established by the US EPA or Germany. The LOQ is a sensitivity which the monitoring for the establishing water quality criteria requires. When the proposed method was used to analyze the target compounds in sixteen surface water samples and total 16 VOCs were detected in surface water samples collected from Gum-River. Maximum concentrations of VOCs detected were not exceeded the EPA or Germany guidelines in any of the samples.

• Analytical Science and Technology
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• v.18 no.4
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• pp.320-328
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• 2005

The most common five chlorophenols (4-chloro-3-methylphenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) were determined from the industrial wastewater by GC/MS. The samples were collected from the petrochemical company, textile company and leather making company. The developed analytical method was modified by USEPA Method 3510. The samples were extracted with dichloromethane under pH 2 and pH 5-6, and determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.9943$) on e ranges of the 0.1 ng/mL~10 ng/mL and 0.5 ng/mL~10 ng/mL, and the limit of detection were between 0.1 ng/mL and 0.5 ng/mL. The absolute recoveries were measured at the concentration of 1, 5, and 10 ng/mL, and the recovery was 71.6~98.9% except for PCP. The relative standard deviation (RSD) was 1.2~14.3% and it gave a good reproducibility for the assay. The bias, which shows the accuracy, was a good although it was a little high values (11.3~22.1%) at the low concentration (1 ng/mL).

• Korean Journal of Environmental Biology
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• v.34 no.3
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• pp.216-221
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• 2016

Level and distribution of fourteen polycyclic aromatic hydrocarbons (PAHs) in the agricultural water samples collected in the waterways located in Gyeonggi and Gangwon, Korea were determined for monitoring and risk assessment. A simplified, fast but effective extraction and clean-up methods combined with gas chromatography tandem mass spectrometry (GC-MS/MS) was employed to measure the concentration of the target compounds. The extraction of the analytes of interest in water sample (10 mL) was performed with acetonitrile (10 mL) and the salt. To purify the target PAHs, the clean-up procedure was employed with 2 mL tubes of dispersive solid phase extraction. The optimized method was validated with recoveries, method detection limit (MDL), accuracy and precision. Good recoveries for each PAHs at 10 and $25{\mu}g\;L^{-1}$ were achieved (60 to 110%, with RSD <20%) with linearity (>0.99). MDL for all the analytes was achieved with $0.2{\mu}g\;L^{-1}$. GC-MS/MS results showed that concentration of phenanthrene in the water samples from Gyeonggi (20 sites) ranged from 0.82 to $2.56{\mu}g\;L^{-1}$ and from Gangwon (15 sites) ranged from 0.83 to $1.62{\mu}g\;L^{-1}$. Other PAHs were not found in the water samples but the continuous monitoring for these areas were required.

• Journal of Life Science
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• v.16 no.6
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• pp.1006-1013
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• 2006

To High Throughput Screening (HTS), a homogeneous fluorescence polarization immunoassay (FPIA) was developed for the quantitative determination of ochratoxin A(OTA) using a $Victor^3$ (PerkinElmer). The homologous tracer, fluorescein-labelled OTA-EDF were synthesized and a specific OTA antibody has been used in the development of the method. It allowed the determination of OTA in the concentration range 0.5-200 ng/ml, with the detection limit of 0.3 ng/ml. The method developed was highly specific and reproducible. OTA spikes in unpolished rice extracts were determinable by FPIA with good recovery. For naturally contaminated unpolished rice samples some disagreement was observed between the results obtained by FPIA and HPLC, which could be related to the a little matrix effect observed for FPIA. Further research is needed to validate the procedure. On the basis of these initial results, this FPIA appears to meet the performance criteria for OTA screening of food samples without a complicated clean-up.

• Journal of Applied Biological Chemistry
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• v.56 no.1
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• pp.53-57
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• 2013

In here, we investigated the quantitative analysis method of indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA) with liquid chromatography-mass/mass spectrometry (LC-MS/MS) or gas chromatography-MS. Two ways of clean-up process were investigated for LC-MS/MS instrumental analysis of IAA, but both a simple dilution and hydrophile-lipophile balance (HLB) solid phase extraction (SPE) were not met the optimal recovery rates for quantitative analysis. On the other hand, the clean-up method for GC-MS was finally optimized through HLB-SPE from 250-folds diluted sample and methylation with trimethylsilyl chloride in methanol for 4 h. The limit of detection for methyl ester of IAA and IBA were both 1.4 mg/L, and recovery rates showed 93-107% from the concentrated liquid fertilizer.

• Journal of the Korean Chemical Society
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• v.40 no.2
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• pp.109-116
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• 1996

A matrix modification was studied for the determination of trace germanium in mineral waters by electrothermal atomic absorption spectrophotometry (ET-AAS). For this, the type and quantity of modifier as well as the use of auxiliary modifier were investigated to realize the efficient modification. Germanium suffers from low sensitivity and poor reproducibility in ET-AAS determination because of the premature loss of germanium via volatile germanium monoxide formation when heated in the presence of carbon. Therefore, the addition of a matrix modifier is necessary to stablize the germanium, thermally and chemically. By the addition of palladium (10 ${\mu}g/mL)$ as a single modifier to the sample containing 500 ng/mL germanium, the charring temperature could be raised from 800 to $1000^{\circ}C$, and its absorbance was also increased, but the atomization temperature was not raised. In this case, the absorbance of germanium was not changed in the range of 10∼70 ${\mu}g/mL$ of palladium added. On the other hand, it was considered that the use of a mixed modifier could modifiy the matrix more effectively than with a single modifier. The best results were obtained by using 1% ammonium hydroxide as an auxiliary modifier together with 10 ${\mu}g/mL$ palladium. The charring temperature could be raised from 800 to $1100^{\circ}C$, without any change of the atomization temperature. With above optimum conditions, the trace amount of germanium in several mineral waters were determined by a calibration curve method, and good recoveries of more than 95% were also obtained in the samples in which a given amount of germanium was spiked. The detection limit of this method was about 6.9 ng/mL.

• The Journal of the Petrological Society of Korea
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• v.24 no.2
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• pp.77-90
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• 2015

The fission track registration techniques for accurate determinations of uranium in solid- and liquid-state geological materials were recommended and their applicability were examined. The determination of uranium can be achieved by optical counting of neutron-induced fission tracks of $^{235}U$ registered on solid-state track detectors under high magnification. In a dry registration method using powdered pellets of rocks (e.g., granite and coal) showing good uranium-affinity, it was not easy to decide an overall mean concentration over the total sample owing to track-clusters caused by frequent presence of uranium-bearing minerals. Separate scanning for homogeneous and track-clustered parts may be an alternative choice. Assuring the homogeneity over the whole sample, high reproducibilities were confirmed both from duplicate detections using mica and Lexan polycarbonate detectors and from multiple measurements at different thermal neutron fluences. The wet registration method using sealed quartz tubes is recommended to overcome the common heterogeneity in uranium concentrations of $10^1ppm$ and more. Adopting the wet registration, the uranium homogeneity was recovered below the $10^0ppm$ level and the lower detection limit was proved to reach without difficulty the $10^2ppb$ (i.e. $ng\;g^{-1}$) level.

• Journal of Environmental Health Sciences
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• v.34 no.4
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• pp.271-278
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• 2008

Dialkylated phthalates have been commonly used as plasticizers and a variety of applications. Phthalate diesters have been shown to be developmental and reproductive toxicants. It is very difficult to exactly estimate the dose of dialkylated phthalates taken up by the general population because of environmental contamination. Urinary metabolites of phthalates enabled to estimate internal exposure. The objective of this study was quantitative determination of phthalate metabolites by LC/MS/MS with on-line cleanup method to analyze phthalate metabolites in Korean children's urine. We employed LC/MS/MS with on-line enrichment and column-switching techniques for this biological monitoring. Metabolites determined were 4 primary metabolites; MEHP, MnBP, MiBP, MEP and 2 secondary metabolites of DEHP; 5-OH-MEHP), 5-oxo-MEHP. We analyzed children's urine from 30 boys and 30 girls. The method detection limit of phthalate metabolites were 0.03 ng/mL for MEP, 1.05 ng/mL for MBP, 0.22 ng/mL for MEHP, 0.15 ng/mL for 5-OHMEHP and 0.16 ng/mL for 5-oxo-MEHP, respectively. Switching Column LC/MS/MS was proven to be a useful tool to determine metabolites of phthalate diesters in human urine. The correlation among phthalate metabolites was very high and statistically significant, except MEP. The children's age (months) was negatively correlated to the concentration of phthalate metabolites. The geometric mean concentration of phthalate metabolites (mg/g creatinine) in children's urine were 25.5 for MEP, 130.3 for MnBP, 56.8 for MiBP, 19.5 for MEHP, 85.6 for 5-OH-MEHP and 83.1 for 5-oxo-MEHP, respectively. Levels of estimated daily intake of parent phthalate compounds (${\mu}g$/kg bw/day) were 0.8 for DEP, 5.0 for DnBP, 1.9 for DiBP and $8.9{\sim}14.2$ for DEHP, respectively. Estimated daily intake for DEP and DiBP were lower than those of other studies but the value for DEHP was higher than that of other study.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.263-268
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• 2019

Methanol is a toxic alcohol used in various products such as antifreeze, detergent, disinfectant and industrial solvent. In the human body, methanol is oxidized to formaldehyde and formic acid, which can lead to metabolic acidosis, optic nerve impairment, and death. In this study, the methanol levels in detergents (n=191) and rinse aids (n=13) were analyzed by gas chromatography-headspace-mass spectrometry (GC-HS-MS). Limit of detection was 1.09 mg/kg, accuracy and precision were 91.1-97.9% and <10%, and it was suitable for quantitative analysis. This analysis method was simple and fast with a higher recovery rate than the conventional MFDS (Ministry of Food and Drug Safety) method of diluting the sample in water and putting it in a headspace vial.

• Analytical Science and Technology
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• v.34 no.1
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• pp.23-35
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• 2021

In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.