• Journal of Life Science
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• v.29 no.2
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• pp.198-201
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• 2019

Recently, it has been reported that Bacillus mojavensis possesses antifungal properties and plant growth-promoting activities, which are similar to the characteristics of siderophore. In this study, the siderophore produced by B. mojavensis was assessed using a solid phase extraction (SPE) cartridge and liquid chromatography quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS). After B. mojavensis was incubated in phenol medium for 16 hr and lyophilized, the sample was dissolved in water and loaded to an SPE cartridge to remove interferences. The cartridge was washed with 5% methanol in water and eluted with 2% formic acid in methanol sequentially. The eluted solution was evaporated under a stream of nitrogen gas and reconstituted in methanol. The reconstituted sample was filtered, and $1{\mu}l$ of the sample was assessed using Q-TOF MS/MS. The mass spectrometer was operated using the positive electrospray ionization mode. Based on the mass spectrum and tandem mass spectrum, the siderophore produced by B. mojavensis was bacillibactin, one of the catechol types of siderophore with a molecular weight of 882.2556. This siderophore analysis could provide a justification for the study of B. mojavensis as a functional food and for pharmaceutical applications.

• YAKHAK HOEJI
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• v.57 no.5
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• pp.330-336
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• 2013

"The Act on Medication Treatment of Sexual Impulse of Sex Offenders" known as chemical castration has been effective since July 2011 in Korea. According to the law, monitoring of male sex hormone in urine is enforced to request National Forensic Service more than once a month after injection of medicine designed to reduce sex impulse. We established a rapid and sensitive method for the monitoring of testosterone (T) and epitestosterone (E) in human urine by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Three mL of urine was pretreated by solid-phase extraction for purification and performed enzymatic hydrolysis. The pretreated samples were extracted twice with 2 ml of ethyl acetate and n-hexane (2 : 3). The separation was applied on Thermo Hypersil GOLD C18 column ($1.9{\mu}m$, $100{\times}2.1mm$). A gradient elution of methanol and water of 0.1% formic acid were used as mobile phase and the retention time was less than 10 min. LC-MS/MS system coupled with an electrospray ionization source was performed in multiple reaction monitoring mode. The transitions of the analytes executed as following: m/z $289{\rightarrow}97$, 109 for T and E, m/z $292{\rightarrow}109$ for $T-d_3$ and $E-d_3$ as internal standards. The validation results of the method were satisfactory. The limits of detection were 0.05 ng/ml and the limits of quantification were 0.1 ng/ml. This method was successfully applied to real human urine sample. The developed method will be useful for monitoring T/E ratio in urine of sex offenders.

• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1783-1790
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• 2013

A simultaneous analytical method has been developed for the fluorimetric determination of haloacetonitriles (HANs) [dichloroacetonitrile (DCAN), trichloroacetonitrile (TCAN), dibromoacetonitrile (DBAN), haloacetamides [dichloroacetamide (DCAD), and trichloroacetamde (TCAD)] in drinking water by using the combined on-line perconcentration/reversed phase liquid chromatography (RPLC)-postcolumn detection system. This on-line perconcentration system was achieved by employing a precolumn packed with a commercial solid phase extraction (SPE) sorbent for the enrichment and purification of the target analytes. The haloacetonitriles and haloacetamides were separated on CN analytical column in a 7.5% methanol-0.02 M phosphate buffered mobile phase at pH 3. The column effluents were reacted with postcolumn reagents of ophthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which were measured with a fluorescence detector. Under the optimized conditions for RPLC and the postcolumn derivatization system all of the coefficient of determination of the standard calibration curves for the target analytes were over 0.99 and had a linear range from 5 to 100 ${\mu}g/L$. The detection limits showed 1.6 ${\mu}g/L$ for DCAD, 0.1 ${\mu}g/L$ for TCAD, 0.6 ${\mu}g/L$ for DCAN, 1.6 ${\mu}g/L$ for TCAN and 1 ${\mu}g/L$ for DBAN, and the recoveries were ranged from 64 to 99% except for DCAD with precisions less than 4.9% in distilled water, and from 72(${\pm}4%$) to 116%(${\pm}2%$) in tap water.

• Analytical Science and Technology
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• v.33 no.3
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• pp.125-133
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• 2020

Methylisothiazolinone (MIT) and chloromethylisothiazolinone (CMIT) cause allergic contact dermatitis and are banned cosmetics ingredients, except in rinse-off products. However, their presence has been detected in cosmetics. We report a UPLC-tandem MS/MS screening method for their simultaneous determination in cosmetics. To facilitate extraction from various matrices, pretreatment methods were developed for each sample type. The method was optimized through a series of assessments, including specificity, LOD, LOQ, linearity, recovery, stability, precision, and accuracy. The LODs and LOQs for MIT ranged from 0.054 and 0.163 ㎍ mL^-1 whereas those for CMIT ranged from 0.040 and 0.119 ㎍ mL^-1. The linear correlation coefficients (r²) were higher than 0.999. Relative standard deviations (RSDs) for both intra- and inter-day measurements ranged from 0.3 ~ 13.6 %. Recoveries at three different concentrations were within 87.9 ~ 118.9 %. The RSD for stability measurements of spiked samples was within 7 %. These results confirm the suitability of the developed method for the simultaneous quantitation of MIT and CMIT in cosmetics. Samples of 320 color cosmetics, including eyeshadows, solid lipsticks, liquid lipsticks, and nail polishes were analyzed using the developed method, and two of them were found to contain both MIT and CMIT and one of them was found to contain only MIT. This data and the method will aid the regulation of ingredients used in cosmetics.

• Journal of Environmental Health Sciences
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• v.36 no.1
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• pp.44-51
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• 2010

This study aimed to develop analytical method for 8-isoprostanes as biomarkers for oxidative stress with LC/MS/MS technique and to apply the method for human urine samples. Analyzed compounds for urinary oxidative stress markers were 7 stereo-isomers of prostaglandins and the internal standard (iso-$PGF_{2{\alpha}}-d_4$) was used to adjust the recovery rate. The method for determining urinary iso-$PGF_{2{\alpha}}$ consisted of solid phase extraction and LC/MS/MS detection. Separation of isomers of prostaglandins completed by porous graphitic carbon column and buffer solution. Detection limits for urinary markers of oxidative stress, iso-$PGF_{2{\alpha}}$ with LC/MS/MS were 0.01 ng/ml by S/N ratio 3 and 0.028 ng/ml by calculated as to FDA method. The recovery (92.8~101.9%) and precision (8.8~20.7%) of analysis were feasible for detecting iso-$PGF_{2{\alpha}}$ in real human urine samples. We detected 4 isomers of prostaglandins in human urine samples. Mean (standard deviation) of urinary iso-$PGF_{2{\alpha}}$ concentration were 0.231 (0.117) ng/mg creatinine for smoking group and 0.154 (0.082) ng/mg creatinine for non-smoking group.

• Korean Journal of Soil Science and Fertilizer
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• v.45 no.1
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• pp.43-50
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• 2012

Two typical animal waste management practices, composting and stockpiling, were evaluated for their effect on the degradation of three veterinary antibiotics (VAs), chlortetracycline (CTC), tylosin (TYL), and monensin (MNS). The VAs were applied to horse manure plots subject to composting or stockpiling, and core samples were collected over a period of time. Selected buffer solutions were used to extract the VAs and analysis for concentration was conducted with solid phase extraction (SPE) followed by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS) technique. The VAs demonstrated rapid dissipation within ten days followed by a gradual decrease in concentration until the end of the experimental period (141 days). All three VAs degraded more rapidly in the composting samples than in the stockpiling samples, particularly between 20 and 60 days of the observation period. Degradation of the three VAs generally followed a first-order kinetic model, and a fitted model with a calculated rate constant was determined for each treatment. TYL in composting showed the fastest degradation, with a calculated rate constant of $0.91day^{-1}$; the slowest degradation was exhibited by MNS in stockpiling, with rate constant of $0.17day^{-1}$. Calculated correlation coefficients ranged from 0.89 to 0.96, indicating a strong correlation between measured concentrations and fitted values in this study. Although concentration of TYL in composting treatment showed below detection limit during the test period, this study suggests that composting can reduce animal waste contaminants prior to field application as fertilizer.

• Korean Journal of Soil Science and Fertilizer
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• v.45 no.6
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• pp.867-876
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• 2012

The concentration of veterinary antibiotics in aqueous and sediment matrices was measured in agricultural irrigation ditches bordering several animal-feeding operations (AFOs) and then compared to its concentration in the watershed. Analytical determination in aqueous samples was based on solid phase extraction (SPE) and appropriate buffer solutions were used to extract residuals in sediment samples. Separation and detection of extracted veterinary antibiotics were performed with high performance liquid chromatograph tandem mass spectrometry (HPLC/MS/MS). In general, higher concentrations of antibiotic were observed in the aqueous phase of irrigation ditches, with the highest concentration of erythromycin hydrochloride (ETM-$H_2O$) of $0.53{\mu}g\;L^{-1}$, than in aqueous watershed samples. In contrast, higher concentrations were measured in river sediment than in irrigation ditch sediment with the highest concentration of oxytetracycline of $110.9{\mu}g\;kg^{-1}$. There was a high calculated correlation ( > 0.95) between precipitation and measured concentration in aqueous samples from the irrigation ditches for five of the ten targeted veterinary antibiotics, indicating that surface runoff could be an important transport mechanism of veterinary antibiotics from field to environment. Further, environmental loading calculation based on measured concentrations in aqueous samples and flow information clearly showed that irrigation ditches were 18 times greater than river. This result suggests the likelihood that veterinary antibiotics can be transported via irrigation ditches to the watershed. The transport via surface runoff and likely environmental loading via irrigation ditches examined in this study helps identify the pathway of veterinary antibiotics residuals in the environment.

• KIEAE Journal
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• v.3 no.1
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• pp.13-20
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• 2003

It is highly recognized that there is need for protection against indoor air pollution, as we realize environmental pollution is growing, For example, in an indoor environment, a person spends more than 80 percent of their time inside the building. Thus, concern about indoor decoration materials is growing, since they cause pollution in the rooms of an apartment, as well as in offices. As the indoor decoration materials become more diverse and lusurious, so the effect of VOCs(Volatile Organic Compounds) and HCHO(Formaldehy) is growing. The indoor decoration materials cause the Sick Building Syndrome, such as headaches, dizziness, or lack of concentraion, and they in turn cause serious deterioration in people's health. In this study, I probed the status of the indoor air pollution and carried on an investigation and analysis about the prevention technique. In doing so, I performed experimental tests and an assessment of the indoor decoration materials of an apartment. I also examined elements of the emitted and the emission. Finally, I examined the character of emissions, by changing environmental conditions, such as the temperature, humidity, and ventilation. With respect to VOCs tests, I applied the method of solid state adsorption using the adsorptive tube, based on the measurement of the American EPA TO-17, ASTM 5116-97, and the measurement of the Japanese Wall Decoration Industrial Association. The tested sample was analyzed by High Performance Liquid Chromatography, after going through the process of dissolvent extraction. As subjects of the test, Paint were selected. The process of this test is as follows; first, I figured out the character of the emission, by measuring the emitted concentration of VOCs and HOHC from the indoor decoration materials of an apartment. Second, I made a small-scale chamber and the test was processed in the chamber in order to suggest an environment-friendly prediction modlel development.

• Korean Journal of Environmental Agriculture
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• v.33 no.2
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• pp.69-77
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• 2014

BACKGROUND: The purpose of this study was to investigate the effects of clothianidin on the soil in terms of clothianidin dissipation and degradation to evaluate its safety in order to provide an analytical foundation for clothianidin and the 5 metabolites related to it. METHODS AND RESULTS: High-performance liquid chromatography(HPLC) was used to separate clothianidin and its metabolites in this study. In soil, after suppressing dissociation-proned ions with weak alkalic $NH_4OH$ and extracting the metabolites with methanol, clothianidin, Methylaminoimidazole(MAI), Methylnitroguanidine(MNG), Thiazolylmethylurea(TZMU) and Thiazolylnitroguanidine(TZNG). Thiazolylmethylguanidine(TMG) were extracted with the addition of neutral $NH_4OAC$ to increasing the intensity of ions. Compounding elements were separated by using Hydrometrix ($ChemElut^{TM}$) and ion-exchanging Solid-phase extraction(SPE) Strong cation-exchanger(SCX) and C18 were used. The recovery rates of clothianidin and 5 metabolites in soil and water ranged from 87.4% to 104.3%. A standard deviation of our analysis for the soil and water samples were less than 5%. CONCLUSION: Well accepted detection limits for clothianidin and 5 metabolites in soil samples based on a dissipation analysis is 0.005 mg/kg and 0.001 mg/L in water samples. The dissipation concentration of this study was decided to be enough to evaluate the dissipation levels of clothianidin and its metabolites.

• Journal of Food Hygiene and Safety
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• v.25 no.1
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• pp.79-82
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• 2010

The pomegranate (Punica granatum), especially its fruit, possesses a vast ethnomedical history and represents a phytochemical reservoir of heuristic medical value. The tree and fruit can be divided into several anatomical compartments, and the fruit juice, peel and oil are known to be weakly estrogenic and heuristically of interest for treatment of menopausal symptoms and sequellae. In this study, analysis of estrogen in pomegranate extract was carried out with LC/MS/MS. Three batches of pomegranate extract samples were used to analysis the target compounds (estrogen). The contents of estrogen derivatives in the samples were 38.6 ppb of estriol, 83.5 ppb of estrone, and 10.9 ppb of estradiol. This result suggests that the pomegranate extract can used for treatment of menopause symptoms in the woman.