• Analytical Science and Technology
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• v.21 no.1
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• pp.41-47
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• 2008

Although liquid-liquid extraction (LLE) method has been used routinely for the analysis of amphetamine-like drugs (amphetamine; AP, methamphetamine; MA, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA), a solid-phase extraction (SPE) method, which can be automated, was applied for the simultaneous determination by GC/MS in human urine. Urine samples (3 mL) and 0.1 M phosphate buffer (1 mL, pH 7.0) were extracted by an automated SPE system. The eluent was evaporated, derivatized with trifluoroacetic anhydride (TFAA), and analyzed by GC/MS. The calibration curves was linear with correlation coefficient ($r^2$) above 0.994 in the ranges of 34.0 (AP), 28.0 (MDA)~1000.0 ng/mL for AP, MDA, and 50.0~2000.0 ng/mL for MA, MDMA, and MDEA. The limits of detection ranged from 4.0 to 10.0 ng/mL, and the limits of quantitation ranged from 12.0 to 34.0 ng/mL. The relative recoveries were 93.5~107.7 %. The precisions and accuracies were 1.9~14.8 % and -8.7~14.8 %, respectively. The present method was successfully applied to identify the MA or Ecstasy (MDMA) abusers in exact as well as rapid.

• Journal of the Korean Society of Marine Environment & Safety
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• v.29 no.4
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• pp.389-394
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• 2023

In recent years, use of machine automation is rising in the industry. Ships also obtain machine condition information from sensor as digital information. However, on ships, crew members regularly surveil the engine room to check the condition of equipment and their information through analog gauges. This is a time-consuming and tedious process and poses safety risks to the crew while on surveillance. To address this, engine room surveillance using an autonomous mobile robot is being actively explored as a solution because it can reduce time, costs, and the safety risks for crew. Analog gauge reading using an autonomous mobile robot requires digitization for the robot to recognize the gauge value. In this study, image processing techniques were applied to achieve this. Analog gauge images were subjected to image preprocessing to remove noise and highlight their features. The center point, indicator point, minimum value and maximum value of the analog gauge were detected through image processing. Through the straight line connecting these points, the angle from the minimum value to the maximum value and the angle from the minimum value to indicator point were obtained. The obtained angle is digitized as the value currently indicated by the analog gauge through a formula. It was confirmed from the experiments that the digitization of the analog gauge using image processing was successful, indicating the equivalent current value shown by the gauge. When applied to surveillance robots, this algorithm can minimize safety risks and time and opportunity costs of crew members for engine room surveillance.

• Journal of Life Science
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• v.34 no.1
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• pp.59-67
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• 2024

LS-RUG-com preparation in a complex extract from mixture of three natural plants. Rubus crataegifolius/unriped, Gardenia jasminoides and Ulmus marcrocarpa that have been widely used in traditional functional health food. This study was conducted to establish the HPLC analysis methods that can be used to establish quantitative analysis of R. crataegifolius, G. jasminoides and U. macrocarpa for standardization of LS-RUG-com preparations. HPLC analysis methods for simultaneous determination of ellagic acid and geniposide and single determination of catechin-7-O-β-D-apiofuranoside were established for the quality control of natural plants complex (LS-RUG-com). Validation of HPLC analysis were performed by checking specificity, accuracy, precision, limit of detection and quantitation, and linearity following ICH (International Council for Harmonisation) guideline. As the result of quantitative analysis, the contents of ellagic acid, geniposide and catechin-7-O-β-D-apiofuranoside in each plant extracts were 11.2 mg/g (ellagic acid) and 72 mg/g (geniposide) and 10.2 mg/g (catechin-7-O-β-D-apiofuranoside). The contents of ellagic acid, geniposide and catechin-7-O-β-D-apiofuranoside in LS-RUG-com were 4.62~6.82 mg/g (ellagic acid), 19.2~28.8 mg/g (geniposide) and 1.36~2.04 mg/g (catechin-7-O-β-D-apiofuranoside) respectively.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.230-240
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• 2015

An IOM sampler equipped with glass fiber filter has been recently utilized instead of solid adsorbent, which was used to measure the inhalation exposure of agricultural operator to pesticides. The aim of this study is to validate the efficacy of an IOM sampler by measuring the trapping efficiency and breakthrough using kresoxim-methyl water-dispersible granule and fenthion emulsifiable concentrate. On LC-MS/ MS, minimum detection level was 12.5 pg and method limit of detection was 5.0 ng/mL. Good linearity ($R^2$ > 0.999) for matrix matched standards was obtained. Recoveries of pesticides from glass fiber filter were 102-109% (kresoxim-methyl) and 97-104% (fenthion) while those from XAD-2 resin were 94-98% (kresoxim methyl) and 93-100% (fenthion). Trapping efficiency test was performed with personal air pumps and IOM sampler (glass fiber filter) connected with solid adsorbent (XAD-2 resin) with two types of formulation (solid and liquid) which were diluted by standard rate and sprayed to IOM sampler. Those pesticides were trapped only in glass fiber filter without any breakthrough to solid adsorbent. After spiking of pesticides to glass fiber filter, breakthrough test was carried out with IOM sampler (glass fiber filter) which was connected with solid adsorbent. As a results, 87-101% of kresoxim-methyl and 96-105% of fenthion remained in spiked glass fiber filter, however, no pesticides were detected in second glass fiber filter and solid adsorbent. In conclusion, IOM sampler which equipped with glass fiber filter can be applied widely for pesticide inhalation exposure study since it has good trapping efficiency and adsorption capacity, regardless of the solid or liquid formulation.

• Analytical Science and Technology
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• v.31 no.4
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• pp.161-170
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• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Journal of Food Hygiene and Safety
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• v.32 no.3
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• pp.187-192
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• 2017

The consumption of herbal medicines has been increasing with growing interest in health. However, due to recent climate change and the complex distribution process of herbal medicines with high import dependence the likelihood of contamination with mycotoxin has been increased. Mycotoxins are emerging as key indicators for ensuring safety of herbal medicines. A total of 498 herbal medicine samples were screened for mycotoxin contamination in this study. Aflatoxin in the herbal medicine samples was extracted by using immunoaffinity column, then the extracted aflatoxin was quantified via high performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) method. The extraction method was verified by linearity, recovery, LOD and LOQ. Aflatoxins were detected in 39/498 samples in an average of $7.670{\mu}g/kg$ ($0.610-77.452{\mu}g/kg$ range). Although safety standards for Corydalis Tuber is not currently available in korea, five of the 39 samples had high concentration of aflatoxins (average of $14.9{\pm}4.1{\mu}g/kg$). In conclusion, it is urgent to establish safety criteria of aflatoxin in Corydalis Tuber. The results of the current study suggest that continuous monitoring is necessary for proactive management of herbal medicine safety.

• Analytical Science and Technology
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• v.29 no.2
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• pp.57-64
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• 2016

Many phthalic acid esters (PAEs), including DMP, DEP, DBP, BBP, and DEHP, as well as DEHA are widely used as plasticizers in plastics. An analytical method was developed and used to analyze these compounds at 41 industrial facilities. The coefficient of determination (R²) for each constructed curve was higher than 0.98. The method detection limit (MDL) values were 0.4–0.7 μg/L for PAEs and 0.6 μg/L for DEHA. In addition, the recovery rate was shown to be 77.0–92.3%, while the relative standard deviation was shown to be in the range of 5.8-10.5%. DMP (n = 3), DEP (n = 2), DBP (n = 2), BBP (n = 2), and DEHA (n = 3) were detected in the range of 2.2-11.1% in the influent. DEHP was a predominant compound and was detected at > MDL in both the influent (n = 16, 35.6%) and the effluent (n = 4, 10.0%) at a high removal efficiency (92–100%). The highest levels of residue in industrial wastewater influent were 137.4 μg/L of DEHP at plastic products manufacturing facility, 12.5 μg/L of DEHA at a chemical manufacturing facility, and 14.0 μg/L of DEP at an electronics facility. The highest concentration of effluent was 12.5 μg/L of DEHP at a chemical manufacturing facility, which indicated that the effluent was below the allowable concentration (800 μg/L). Therefore, the levels of PAEs and DEHA that are discharged into nearby streams could not influence the health of the ecosystem.

• Analytical Science and Technology
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• v.31 no.2
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• pp.96-105
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• 2018

This study aimed to improve the method for detecting eight secondary aliphatic amines (SAAs), so as to measure their concentrations in fresh water and tap water samples. NaOH (8 mL, 10 M) and benzenesulfonyl chloride (2 mL) were added to a water sample (200 mL), and the mixture was stirred at $80^{\circ}C$ for 30 min. An additional NaOH solution (10 mL) was added and the stirring was continued for another 30 min. The pH of the cooled mixture was adjusted to 5.5-6.0 by adding HCl (35 %), and the SAAs were extracted using dichloromethane (50 mL). This extraction was repeated once. The extract was then washed with $NaHCO_3$ (15 mL, 0.05 M) and dried over $Na_2SO_4$ (4 g). The extract was finally concentrated to 0.1 mL, of which $1{\mu}L$ was analyzed for SAAs by GC-MS. The linearity of the spike calibration curves was high ($r^2=0.9969-0.9996$). The detection limits of the method ranged from 0.01 to $0.20{\mu}g/L$, and its repeatability and reproducibility (expressed as relative standard deviation) were both less than 10 % (6.6-9.4 %). Its accuracy (measured in percentage error) ranged between 2.4 % and 6.1 %. The established method was applied to the analysis of five surface water and 82 tap water samples. Dimethylamine was the only SAA detected in all the water samples, and its average concentration was $0.79{\mu}g/L$ (range: $0.20-2.54{\mu}g/L$). Therefore, this study improved the analytical method for SAAs in surface water and tap water, and the regional and seasonal concentration distributions were obtained.

• Journal of Korean Society of Environmental Engineers
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• v.28 no.2
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• pp.158-164
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• 2006

Offensive odor from CAFO(concentrated animal feeding operation) and its control have become a significant issue in Korea. Control of odors from the CAFO requires to identify major odorant and their generation mechanisms. In this study, an easy method to collect gas sample and to quantify its odorants is proposed. The method involves on-site odorant extraction with solid-phase microextraction and quantitation with GC/MSD or GC/FID. Analytes of the current study include: trimethylamine(TMA), carbon disulfide($CS_2$), dimethyl sulfide(DMS), dimethyl disulfide(DMDS), acetic acid(AA), propionic acid(PA) and n-butyric acid(BA). The resulting linearity($R^2$) of calibration curve for each analyte was good over the range from several ppbv to ppmv; 0.984 for TMA(0.056-1.437), 0.996 for $CS_2$(0.039-0.999), 0.994 for DMS(0.029-0.756), 0.995 for DMDS(0.024-0.623), 0.992 for AA(0.068-1.314), 0.955 for PA(0.047-0.940), and 0.976 for BA(0.036-0.712). Method detection limits were 5.67, 6.39, 5.78, 25.2, 0.098, 0.363 and 0.099 ppbv for AA, PA, BA, TMA, DMS, $CS_2$, and DMDS, respectively. With the developed method, odorants from poultry, swine, and cattle barns were analysed. All the compounds but DMDS were detected from the sample collected in the poultry barn, and their levels exceeded the representative published human olfactory threshold.

• Korean Journal of Food Science and Technology
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• v.52 no.4
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• pp.317-324
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• 2020

In order to create the national food nutrient database, a total of 41 animal foods (ham, seafood, edible insects and eggs) were analyzed for their vitamin B₁₂ content and the applied immunoaffinity-HPLC was verified. Ham vitamin B₁₂ contents were 0.30-0.65 ㎍/100 g. Seafood showed relatively high vitamin B₁₂ level, where the values of fermented clam were the highest (26.80 ㎍/100 g) followed by fermented pollack roe. Vitamin B₁₂ was not detected in silkworm pupae and beetles, while relatively high levels were found in the two-spotted cricket imago (6.70 ㎍/100 g). Chicken and quail egg yolk had roughly 100- and 30-times higher vitamin B₁₂ levels as compared to their egg white. Vitamin B₁₂ contents in quail and chicken eggs were significantly enhanced by boiling (p<0.05). Results based on accuracy (97-102% recovery) and precision (<5% RSD) indicate that this study provides reliable vitamin B₁₂ information on animal foods consumed in Korea.