• Bulletin of the Korean Chemical Society
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• v.32 no.3
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• pp.809-814
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• 2011

A method based on the TMS derivatives and acidic hydrolysis was developed for the simultaneous determination of free and conjugated steroidal hormones in surface water. A silylation of five natural and two synthetic steroidal hormones was achieved with N-methyl-N-(trimethylsilyl) trifluoroacetamide/$NH_4I$ (1000:3) under catalysis of dithioerythritol for 60 min at $80^{\circ}C$. TMS derivatives of the steroid hormones containing multifunctional groups offer a single derivative product under this condition. The accuracy of the analytes was in the range of 87 to 110% at a concentration of 20 and 50 ng/L with relative standard deviations of less than 10%. The method detection limit was in the range of 0.01 to 0.02 ng/L for surface water. Natural steroidal hormones were detected in a concentration range of 0 to 1.03 ng/L in free form and 0 to 14.6 ng/L in conjugated form, respectively. We found that most of the natural hormonal steroids exist in conjugate forms (43 to 100%) in river water.

• Journal of Korean Society of Environmental Engineers
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• v.32 no.6
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• pp.615-624
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• 2010

The aims of this study were to investigate and confirm the occurrence and distribution patterns of synthetic musk compounds (SMCs) in Nakdong river basin (mainstream and its tributaries). 4 (HHCB, AHTN, AHMI and ADBI) out of 6 polycyclic musk compounds (PMCs) and 1 (musk xylene, MX) out of 5 nitro musk compounds (NMCs) were detected in 29 sampling sites and HHCB (>50%) was predominant compound followed by musk ketone (MK) and AHTN. The total concentration levels of SMCs on February 2009 and on September 2009 in surface water samples ranged from N.D. to 2147 ng/L and N.D. to 1386 ng/L, respectively. The highest concentration level of SMCs in the mainstream and tributaries in Nakdong river were Goryeong and Jincheon-cheon, respectively. The sewage treatment plants (STPs) along the river affect the SMCs levels in river and the SMCs levels decreased with downstream because of dilution effects.

• Analytical Science and Technology
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• v.25 no.4
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• pp.242-249
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• 2012

Total 11 samples of sediments from the Geum river and the Nakdong river and its estuaries were analyzed to investigate the distribution characteristics of PBDEs and HBCD. Concentration of PBDEs in sediments ranged from 2.19~101.34 (average 30.70, median 20.91) ng/g-dw. The concentration range of PBDEs in river sediments is greater than those of estuary sediments. The HBCD concentration was ranged from N.D.~7.85 (average 1.47, median 0.32) ng/g-dw. HBCD concentrations compared with PBDEs are approximately 1/20 level, which is associated with low domestic usage. Isomer patterns of PBDEs and HBCD suggested that not only the use of commercial products, but the physicochemical properties of these materials, environmental degradation, and environmental behavior could affect the distribution characteristics of these chemicals and their isomers.

• Journal of Life Science
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• v.10 no.3
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• pp.247-253
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• 2000

The effects of acute of marine toxicants on early life of coastal olive flounder were investigated. An increasing order of acute toxicity on embryo- and larva-stages of Paralichtys olivaceus was CdCl2$\mu\textrm{g}$/L and 29 $\mu\textrm{g}$/L, respectively, and those values at larva-stage were estimated 3.5 ng/L, 16.0 nL/L, 10.5 $\mu\textrm{g}$/L and 15.0 $\mu\textrm{g}$/L, respectively.

• Analytical Science and Technology
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• v.15 no.3
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• pp.300-316
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• 2002

The extraction methods of PBBs from environmental samples by soxhlet extraction for solid phase and liquid-liquid extraction for liquid phase were compared. After extraction, silicagel and florisil as column clean up methods were used for the comparison of cleanup efficiency with different solvent system. Also, the analytical instruments were used GC/MSD. The 22 kinds of PBBs standards were used to establish the analytical methods to perform the experiments of recoveries and detection limits in water and soil. The detection limits of PBBs represented 5~10 ng/L for water and 0.5~3.5 ng/g for soil samples, respectively. The recoveries of water samples represented 96~107% in n-hexane, dichloromethane and toluene for water, and 60~80% in combined solvent with n-hexane and acetone. The recoveries of soil sample were surveyed 67~97% in soxhlet extraction and 64~76% in ultrasonic extraction with selected solvents.

• YAKHAK HOEJI
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• v.48 no.3
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• pp.207-212
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• 2004

An analytic method was developed for the quantitation of $\Delta$$^{9}-$ tetrahydrocannabinol (THC) and 11-nor-9-carboxy THC (THC-COOH) in human hair. After hair samples were pulverized using Freezer Mill, deuterated internal standards were added and digested in 1 N NaOH at $100^{\circ}C$ water bath for 30 min. Digest solutions were extracted by 5 ml hexane：ethyl acetate (90：10) after acidification with acetic acid. The organic phase was evaporated under N 2 and derivatized by BSTFA (with 1% TMCS) at $85^{\circ}C$ for 45 min. The derivatized solution was separated on HP-5MS column ($30m{\times}0.25mm{\times}0.25mm$) and detected using EI-GC-MS with selective ion monitoring mode. The assay of calibration was ranged from 5 to 100 ng/50 mg hair ($r^2$＞0.99) for THC and THC-COOH. Within and between-run precision were calculated at 6, 30, 60 ng/50 mg hair with coefficients of variation less than 11%. Within and between run accuracies at the same concentrations were$\pm$14% and $\pm$30% of target for both analytes, respectively. Absolute and relative recovery at 10 and 100 ng were 60∼91％. The method was used to detect and quantify THC and THC-COOH in cannabis abuser's hairs (N = 16) and SRM (N=5, THC 1 ng/mg, NIST). We detected THC and THC-COOH in only one hair sample. In SRM, % accuracy was 93% (range 86∼103%) and precision (% CV) was 8.14. We began to set up a quantitative analysis of THC and THC-COOH using EI-GC-MS. Continuously, we need to modify and develop this method in order to apply for identification in cannanbis users' hair.

• 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.

• Analytical Science and Technology
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• v.15 no.6
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• pp.534-539
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• 2002

We established an analytical method for the measurement of trace amounts of earthy/musty odorous geosmin (GSM) and 2-methylisoborneol (2-MIB) in water using GC/MS. Water samples were extracted with n-hexane (liquid-liquid extraction, LLE) and the extracts were measured by GC/MS. The extraction yields of the two compounds were tested to be ($87{\pm}8$)% and ($78{\pm}8$)%, respectively. The limits of quantitation (LOQs) of the two compounds by this method were greatly improved to ~0.3 ng/L. The analytical methods were applied to analyze water samples from several rivers in Korea and waters after water treatment processes. The highest levels of geosmin and 2-methylisoborneol in raw water from a river were measured to be ($4.2{\pm}0.4$) ng/L and ($44{\pm}4$) ng/L, respectively. The levels only slightly decreased to ($1.3{\pm}0.1$) ng/L and ($18{\pm}2$) ng/L even after water treatment, indicating that the odorous compounds were not properly removed by the treatment processes.

• Asian-Australasian Journal of Animal Sciences
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• v.16 no.6
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• pp.823-829
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• 2003

Four different types of silage from new cultivars of Napier grass (Pennisetum purpureum), cv. NG 1 and NG 2, were fed to eight wethers in order to evaluate their preference and intake by sheep. The silages were prepared from direct-cut NG 1 herbage; pre-wilted NG 1 herbage; NG 1 herbage with maize meal (5% inclusion) and NG 2 herbage with maize meal (5% inclusion). All silages were palatable to sheep. Maize-treated silage had high quality fermentation, characterized by high Fleig scores and low pH, volatile fatty acids (VFA) and ammoniacal nitrogen contents. The pH, Fleig score, in vitro digestible organic matter (IVDOMD) and ammoniacal-N contents for maize-treated cv. NG 1 silage were 3.7, 78, $540g\;kg^{-1}$ dry matter (DM ) and $0.18g\;kg^{-1}$ DM whereas, in maize-treated cv. NG 2 they were 3.6, 59, $^458g\;kg{-1}$ DM and $0.18g\;kg^-1$ DM, respectively. The superior quality of maize-treated silages made them more preferable to sheep. Among the maize-fortified silages, palatability and intake were significantly (p<0.001) greater with cv. NG 1. Although direct-cut silage had better fermentation quality compared to wilted silage, wilted silage was significantly (p<0.001) more preferable to sheep. However, there were no significant differences (p<0.05) in the levels of preference and intake of wilted silage compared to maize-treated cv. NG 2 silage, even though the latter tended to be more palatable. There were indications that high pH (4.6 vs 3.5) and IVDOMD content (476 vs $457g\;kg^{-1}%$ DM) of wilted silage contributed to higher intake, compared to direct-cut silage. It was generally concluded that pre-wilting and treatment of Napier grass with maize meal at ensiling enhances intake and palatability.

• Analytical Science and Technology
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• v.17 no.1
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• pp.69-81
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• 2004

The formation pattern of DBPs (disinfection by-products) in raw water treated with hypochlorite, chlorine disinfectant was studied. TOC (total organic carbon), residual chlorine, turbidity and 14 DBPs in raw water from Han-river and Nakdong river during 1 ~ 14 days were determined. Total DBPs in Han river was 101.3 ng/mL (789.6 nM) after 7days and THMs (trihalomethanes) are the dominant portion of 68%. HAAs (haloacetic acids) and chloral hydrate were determined 19% and 10% respectively. In Nakdong river total DBPs was 98.4 ng/mL (678.6 nM) and dominant class was HAAs. (55.8 ng/mL, 57%) THMs(34%) and N-compounds like HANs (haloacetonitriles, 5%) and chloropicrin were increased. It may be explained that high concentration of NH4-N in Nakdong river react with chlorine produced chloramine and this formed different pattern of DBPs. As a result, total DBPs formation pattern depends on raw water and disinfectant and in generally the initial concentration of acidic HAAs was high and THMs was increased gradually.