• Journal of Korean Society of Water and Wastewater
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• v.32 no.5
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• pp.389-398
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• 2018

A nationwide survey of 8 N-nitrosamines in finished water samples from drinking water treatment plants (DWTPs) in Korea was conducted. The samples were pre-treated by solid-phase extraction (SPE) and analyzed using a gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). According to the study results, four N-nitrosamines (NDMA, NDEA, NMOR, NDBA) were detected for three consecutive years, NMEA and NPYR were only found in samples collected in 2013. Two of these N-nitrosamines, N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA), have received attention and were the most commonly detected. The concentration of NDMA and NDEA in this study ranged from $0.002{\mu}g/L$ to $0.013{\mu}g/L$ and in $0.001{\mu}g/L$ to $0.008{\mu}g/L$, respectively. In comparison to studies performed in EPA(UCMR2), the concentrations of NDMA (from $0.002{\mu}g/L$ to $0.630{\mu}g/L$) and NDEA (from $0.005{\mu}g/L$ to $0.100{\mu}g/L$) observed in the this study were low.

• Journal of Environmental Health Sciences
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• v.40 no.6
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• pp.435-441
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• 2014

Objectives: Bisphenol A, or BPA, is a chemical component in polycarbonate plastic with which many people come into contact every day. A great deal of controversy has arisen over its safety since this material, which is known to disrupt the human endocrine system and cause neurological difficulties and cancer, is commonplace in beverage containers, food can liners, and receipt paper rolls. In this study, we determined the levels of exposure to BPA of workers in the service industry depending on the number of receipts contacted. Methods: The participants were 16 male and 18 female workers employed in the service industry. Using a questionnaire, we investigated general and job characteristics. Urine samples were collected and analyzed by the LC-MS/MS technique after enzymatic hydrolysis and solid phase extraction (SPE). Results: The geometric mean (GM) concentration of urinary BPA from all subjects was 1.02 ng/ml. Workers were exposed significantly to more BPA according to the number of receipts they contacted, their work experience, and working hours per day. The BPA concentration of those who touched more than 100 receipts per day was 3.09 ng/ml, while that of the other participants was 0.61 ng/ml. It was shown that wearing gloves can protect from BPA exposure. Conclusion: We determined the urinary BPA concentrations of workers in service industry and found that the contact with receipts could increase the BPA exposure of service workers.

• Bulletin of the Korean Chemical Society
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• v.33 no.11
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• pp.3665-3670
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• 2012

Metal-p-$NH_2$-Bn-DOTA (paraammionobenzyl-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid: ABDOTA) complex was synthesized and purified for bio-tagging to quantify biological target materials using laser ablation (LA)-ICP-MS. Since the preparation of a pure and stable tagging complex is the key procedure for quantification, magnetic particles were used to purify the synthesized metal-ABDOTA complex. The magnetic particles immobilized with the complex attracted to a permanent magnet, resulting in fast separation from free un-reacted metal ions in solution. Gd ions formed the metal-complex with a higher yield of 64.3% (${\pm}3.9%$ relative standard deviation (RSD)) than Y ions, 52.3% (${\pm}2.5%$ RSD), in the pH range 4-7. The complex bound to the magnetic particles was released by treatment with a strong base, of which the recovery was 81.7%. As a reference, a solid phase extraction (SPE) column packed with Chelex-100 resin was employed for separation under similar conditions and produced comparable results. The tagging technique complemented polydimethylsiloxane (PDMS) microarray chip sampling in LA-ICP-MS, allowing determination of small sample volumes at high throughputs. For application, immunoglobulin G (IgG) was immobilized on the pillars of PDMS microarray chips and then tagged with the prepared Gd complex. IgG could then be determined through measurement of Gd by LA-ICP-MS. A detection limit of 1.61 ng/mL (${\pm}0.75%$ RSD) for Gd was obtained.

• Korean Journal of Veterinary Service
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• v.25 no.1
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• pp.23-29
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• 2002

A method was developed to separate, detect and qualify aldicarb, bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur in meats and fruits. Experimental beef and fork samples were fortified with 0.05mg/kg of carbamate pesticides for analysis. Carbamate-detected pear by HPLC fluorescence detector(HPLC/FLS) are extracted with acetonitril and refined by solid phase extraction(SPE) filled with aminopropyl-bonded silca, In the following step, the injected materials into LC/MS are analyzed to result in the fact that bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur presents several sorts of fraction ions following with; [M+H]$^{+}$, [M+Na]$^{+}$,［M-CONH$CH_3$]$^{+}$, [M-OCONH$CH_3$]$^{+}$. In addition, ethiofencarb presents [M-SCH$_2$$CH_3$]$^{+}$ ion distinctive and aldicarb presents [M+Na]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ ion which is the most decisive fraction ion for pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur excluding [M+H]$^{+}$ ion. However, [M-OCONH$CH_3$]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ fraction ion charactering carbamate pesticides are detected most efficiently with fragment voltage 50ev. As a result, for rluantitative analysis, [M+Na]$^{+}$ ion is the most decisive ion for detection of aldicarb and [M+H]$^{+}$ ion is the most decisive fraction ion for Pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur. Carbaryl-detected pear by HPLC/FLS are analyzed by L/MS and the result shows that [M+H]$^{+}$ and [M-CONH$CH_3$]$^{+}$ ions charactering carbaryl are detected.ering carbaryl are detected.

• YAKHAK HOEJI
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• v.52 no.6
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• pp.480-487
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• 2008

We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH), the major metabolite of ${\Delta}^9$-tetrahydrocannabinol, in urine sample by solid-phase extraction (SPE) and GC/MS detection. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day and inter-person validation were performed using statistical analysis of several indicative factors. Measurement uncertainty associated with target analyte in real forensic samples was estimated using quality control (QC) data. Traceability of measurement was established through traceable standards, calibrated volumetric glassware and volume measuring device. The major factors of contribution to combined standard uncertainty, were calibration linearity, inter-day repeatability and inter-person reproducibility, while those associated with preparation of analytical standards and sampling volume were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method was 12.05% for THCCOOH.

• Korean Journal of Soil Science and Fertilizer
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• v.49 no.3
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• pp.242-250
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• 2016

Veterinary antibiotics (VAs) has been used to treat animal disease and to increase animal weight as growth promoter. However, abused usage of VAs can cause production of antibiotic resistance genes (ARGs) in the environment and additionally, residual of VAs in soil can be transferred into crops. Therefore, main objective of this research was to examine bioaccumulation of VAs in sprouts (red cabbage, Brassica Olearacea L. var. Capitata f. rubra and red radish, Raphanus sativus) with hydroponic method. Total of 7 VAs in 2 different classes of VAs (tetracyclcines: tetracycline, oxytetracycline, chlortetracycline, sulfonamides: sulfamethoxazole, sulfamethazine, sulfamethiazole, macrolides: tylosin) were evaluated and experiment was conducted with solid phase extraction (SPE)/high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). Initial spiked concentration of 7 VAs was $5mg\;L^{-1}$ and cultivation period was 8 days. Result showed that growth of sprouts was inhibited about 23-27% when VAs was introduced. Amount of bioaccumulated VAs was also differed depending on class of VAs. The highest amount of bioaccmulated VAs was tetracycline and sulfamethoxazole in each class with a concentration of 4.05, $7.73mg\;kg^{-1}$ respectively. Calculated transfer ratio of VAs into crops was also ranged 0.38-54.27%. Overall, bioaccumulation of VAs in crops can be varied depending on crop species and class of VAs. However, further research should be conducted to verify bioaccumulation of VAs in crops in the soil environment.

• Analytical Science and Technology
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• v.17 no.1
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• pp.29-36
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• 2004

An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

• The Korean Journal of Pesticide Science
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• v.16 no.4
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• pp.273-281
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• 2012

This study was conducted for the establishment of the analytical method of pesticide residues in rice straw for 9 pesticides; etofenprox, tricyclazole, diazinon, edifenphos, propiconazole, carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran and for the monitoring of these pesticides in rice straw for livestock feed in Korea. These pesticides were classified into 4 groups according to analytical instrument condition. Group 1 (HPLC-UVD1) included tricyclazole and etofenprox while group 2 (HPLC-UVD2) included propiconazole and edifenphos. Group 3 (HPLC-FLD) included carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran. Group 4 (GC-NPD) included Diazinon. The dried rice straw samples were extracted with acetone and purified by liquid-liquid partition and solid phase extraction (SPE): Combination of Florisil SPE and amino-propyl SPE was used for group 1 and group 2, amino-propyl SPE for group 3, and Florisil SPE was for group 4. Recovery was in the ranged 70~110% and the limits of quantitation (LOQ) were lower than the half of maximum residue limits. Therefore this method was proved to be efficient for monitoring of these pesticides residue in rice straw. A total of 18 rice straw samples from 6 provinces in Korea in 2010 were analyzed using established method and, only 3-keto carbofuran was detected in one sample at concentration of 0.04 mg/kg.

• Korean Journal of Food Science and Technology
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• v.47 no.5
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• pp.556-560
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• 2015

This study was aimed at investigating the natural occurrence of caffeine, theobromine, and theophylline in tea leaves. Sample clean-up was based on a simple solid phase extraction (SPE) treatment, and simultaneous analysis was performed by high performance liquid chromatography (HPLC). This method showed good results in terms of linearity, recovery, precision, limit of detection (LOD), and limit of quantitation (LOQ). The caffeine, theobromine, and theophylline contents of tea leaves (n = 228) ranged from 5.4 to 58.2 mg/g, from not detected to 11.2 mg/g, and from not detected to 0.7 mg/g, respectively. The results obtained in this study can be used as fundamental data of caffeine, theobromine, and theophylline contents in tea leaves.

• Analytical Science and Technology
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• v.23 no.5
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• pp.437-445
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• 2010

The aim of this study was to develop an analytical method for sulfonamide antibiotics (sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfathiazole) and their metabolites ($N^4$-acetylsulfadiazine, $N^4$-acetylsulfamerazine, $N^4$-acetylsulfamethazine, $N^4$-acetylsulfamethoxazole, sulfamethoxazole-$N^1$-glucuronide) in environmental samples. The solid phase extraction (SPE) with LC/ESI-MS/MS have been used for the analysis of target compounds, and the recoveries of SPE clean-up were at the range of 12-94% for C18 cartridge, 60-95% for HLB cartridge, 25-123% for MCX cartridge, and 70-90% for tandem HLB/MCX. By established method, detection limit, recovery, and relative standard deviation were 0.001~0.187 ng/mL, 66~115%, and 5~17%, respectively. This method was effective and sensitive to use for the simultaneous determination of sulfonamide antibiotics and their metabolites in environmental samples. Four sulfonamide antibiotics were detected at the range of 0.008~2.153 ng/mL. For metabolites, only $N^4$-acetylsulfamethoxazole was detected, but the concentration was under the MDL level.