• Analytical Science and Technology
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• v.20 no.1
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• pp.84-90
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• 2007

To determine levels of 11 sulfonamides for animals in food, simultaneously, a selective method of high performance liquid chromatography with UV detector has been applied. The targets were sulfachlorpyridazine (SCP), sulfadiazine (SDZ), sulfadimethoxine (SDM), sulfisoxazole (SSX), sulfamerazine (SMZ), sulfamethazine (SMT), sulfamethoxazole (SMX), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfaquinoxaline (SQX) and sulfathiazole (STZ). Food samples were beef, pork, chicken, milk and whole egg that were collected at the main 6 cities in Korea as Seoul, Busan, Daejon, Incheon, Mokpo and Gangneung. After homogenizing food samples with sodium phosphate solution and acetonitrile, it was extracted with n-hexane. The mobile phase gradient was a mixture of 5 mM potassium phosphate (pH 3.25) and methanol with a gradient ratio from 100:0 to 30:70. The UV wavelength was 270 nm. The overall recoveries were ranged from 75% to 95% and the limit of detection was minimum 0.004 mg/kg for SMT, and 0.007 mg/kg for STZ at signal/noise > 3, respectively. As results, sulfonamide drugs were not detected in most of the selected food samples, however, sulfamonomethoxine was detected in meat. The determined level of sulfamonomethoxine were 0.03 and 0.06 mg/kg for beef that were below the MRLs.

• Analytical Science and Technology
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• v.19 no.2
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• pp.142-148
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• 2006

To determine malachite green and leuco-malachite green residues in sea food, a liquid chromatographic method has been optimized. The target compounds were extracted in the homogenized edible tissues with a mixture of McIlvaine buffer-acetonitrile and partitioned against dichloromethane. After concentrating the lower layer, the resulting residues were re-dissolved in methanol and analyzed by the HPLC with visible detector at 620 nm using acetonitrile-acetate buffer. For the analysis of leuco-malachite green with malachite green simultaneously, post-column packed with lead(IV) oxide was used for oxidizing leuco-malachite green to malachite green. The correlation coefficients($r^2$) was 0.9989 for malachite green, and 0.9995 for leuco-malachite green. The limit of detection was 0.005 mg/kg for the combined of malachite green and leuco-malachite green at signal/noise${\geq}3$. The recovery rate was within a reliable range of 84~98% (CV 3~16%). Leuco-malachite green were detected in carp and crusian carp.

• Analytical Science and Technology
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• v.22 no.5
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• pp.360-368
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• 2009

Tributyltin (TBT) use has been prohibited by the IMO (International Maritime Organization), as well as Korea, since 2003. This prohibition has affected a gradual reduction in TBT use in maritime environs (seawater, sediment, and biosamples) in several countries. In this study, Crassostrea gigas (oyster) and Tapes philippinarum (manila clam) were chosen and measured for butyltin compound concentrations to verify TBT pollution levels since its 2003 ban. Specimens were taken directly from farms for concentration measurement, where Crassostrea gigas and Tapes philippinarum are cultivated, as well as prevalent locations predicted to have been polluted. Concentrations of MBT, DBT, and TBT of Crassostrea gigas were measured to be N.D -N.D., N.D. -N.D., and N.D. -60.21 ng Sn $g^{-1}$ (wet wt), respectively. Regarding Tapes philippinarum, MBT, DBT, and TBT were N.D. -12.27 ng Sn $g^{-1}$ (wet wt), N.D. -45.95 ng Sn $g^{-1}$ (wet wt), and N.D.-7.30 ng Sn $g^{-1}$ (wet wt), respectively. For this research, a correlative study was conducted to determine butyltin compound concentration in Crassostrea gigas at the locations where measurements were made in 1994 to determine to what extent TBT pollution level decreased. A decrease in all 7 sites was observed. In 4 of the 7 samples, butyltin compounds were measured to be below the detection limit, while that of the Tapes philippinarum did not appear high compared to foreign research data.

• Analytical Science and Technology
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• v.21 no.6
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• pp.518-525
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• 2008

Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

• Analytical Science and Technology
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• v.15 no.4
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• pp.329-334
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• 2002

Tributyl phosphate(TBP) is used in solvent extraction process for radioactive waste. This compound may be degraded to dibutyl phosphate($DBP^-$), monobutyl phosphate($MBP^{2-}$) and ${PO_4}^{3-}$ by radioactive material. Amount of $DBP^-$ and $MBP^{2-}$ in TBP must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for $DBP^-$, $MBP^{2-}$, $F^-$, $Cl^-$, ${NO_2}^-$, ${NO_3}^-$, ${SO_4}^{2-}$ and ${PO_4}^{3-}$ are studied with AS4A-SC(Dionex) analytical column and $Na_2CO_3$/NaOH eluent by Ion chromatography. Optimum condition for these anions is 2 mM $Na_2CO_3$/1 mM NaOH eluent. All anions by this condition is well separated within 15min. Dynamic range is $10{\mu}g/mL$ - $100{\mu}g/mL$ for DBP and $5{\mu}g/mL$ - $50{\mu}g/mL$ for $MBP^{2-}$, respectively. The Detection limit for AS4A-SC are $1{\mu}g/mL$ for $DBP^-$ and $0.5{\mu}g/mL$ for $MBP^{2-}$ in this system with a $25{\mu}L$ sample loop.

• 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).

• Analytical Science and Technology
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• v.18 no.3
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• pp.201-205
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• 2005

Tri-octyl amine (TOA) is used in solvent extraction process for radioactive waste. This compound may be degraded to di-octyl amine (DOA), mono-octyl amine (MOA) by radioactive materials. Amount of TOA, DOA and MOA in TOA must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for TOA, DOA and MOA are studied with Phenomenex LUNA-$C_{18}$ ($4.6mm{\times}25cm$) analytical column and $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) eluent by liquid chromatography. Optimum condition for these compounds is $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) = 85 : 15 ratio. TOA, DOA and MOA compounds is well separated within 20 minute. Dynamic range is $30{\sim}160{\mu}g/mL$ for TOA, $5{\sim}100{\mu}g/mL$ for DOA and $0.1{\sim}5{\mu}g/mL$ for MOA, respectively. The detection limit are $0.1{\mu}g/mL$ for TOA, $1{\mu}g/mL$ for DOA (in SCAN mode) and $0.1{\mu}g/mL$ for MOA (in SIM mode) in this system with $20{\mu}L$ sample loop.

• The Journal of Korean Institute of Communications and Information Sciences
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• v.33 no.2C
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• pp.192-199
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• 2008

In ultra-wideband (UWB) systems, conventionally, the synchronization is to align time phases of a locally generated template and any of multipath components to within an allowable range. However, the synchronization with a low-power multipath component could incur significant performance degradation in receiver operation (e.g., detection) after the synchronization. On the other hand, the synchronization with a high-power multipath component can improve the performance in receiver operation after the synchronization. Generally, the first one among multipath components has the largest power. Thus, the synchronization with the first path component can make better performance than that with low-power component in receiver operation after the synchronization, Based on which, we first propose an optimal decision rule based on a maximum likelihood (ML) approach, and then, develope a simpler suboptimal decision rule for selecting the first path component. Simulation results show that the system has good demodulation performance, which uses new synchronization definition and the proposed decision rules have better performance than that of the conventional decision rule in UWB multipath channels. Between macroblocks in the previous and the current frame. On video samples with high motion and scene change cases, experimental results show that (1) the proposed algorithm adapts the encoded bitstream to limited channel capacity, while existing algorithms abruptly excess the limit bit rate; (2) the proposed algorithm improves picture quality with $0.4{\sim}0.9$dB in average.

• Korean Chemical Engineering Research
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• v.60 no.1
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• pp.1-6
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• 2022

As the demand for wearable devices increases, many studies have been studied on the development of flexible electrode materials recently. In particular, the development of high-performance flexible electrode materials is very important for wearable sensors for healthcare because it is necessary to continuously monitor and accurately detect body information such as body temperature, heart rate, blood glucose, and oxygen concentration in real time. In this study, we fabricated the nonenzymatic glucose sensor based on polyaniline/carbon nanotube fiber (PANI/CNT fiber) electrode. PANI layer was synthesized on the flexible CNT fiber electrode through electrochemical polymerization process in order to improve the performance of a flexible CNT fiber based electrode material. Surface morphology of the PANI/CNT fiber electrode was observed by scanning electron microscopy. And its electrochemical characteristics were investigated by chronoamperometry, cyclic voltammetry, electrochemical impedance spectroscopy. Compared to bare CNT fiber electrode, this PANI/CNT fiber electrode exhibited small electron transfer resistance, low peak separation potential and large surface area, resulting in enhanced sensing properties for glucose such as wide linear range (0.024~0.39 and 1.56~50 mM), high sensitivity (52.91 and 2.24 ㎂/mM·cm²), low detection limit (2 μM) and good selectivity. Therefore, it is expected that it will be possible to develop high performance CNT fiber based flexible electrode materials using various nanomaterials.

• Analytical Science and Technology
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• v.17 no.6
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• pp.520-526
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• 2004

To determine 6 anti-impotence drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil and hongdenafil in food, simultaneously, high performance liquid chromatography was applied. In the case of solid sample, it was extracted in organic solvents after homogenizing with mortar and pestle. Whereas liquid sample was just diluted in water and then extracted in organic solvents. Maximum lengths of UV for targets have been identified on photodiode array spectra. As results, vardenafil, hongdenafil, hydroxyhomosildenafil, sildenafil, homosildenafil, and tadalafil were eluted in order using $C_{18}$ column in acetonitrile containing phosphoric acid as the mobile phase. The maximum wavelength (${\lambda}_{max}$) was 216 nm for vardenafil, 233 and 282 nm for hongdenafil, 222 and 293 nm for hydroxyhomosildenafil, sildenafil and homosildenafil, and 284 nm for tadalafil. The overall recoveries were ranged from 95% to 109% and the limit of detection was about 0.04 mg/kg at signal/noise>3. Levels of targets in the selected food samples were 1.7 (hongdenafil) ~ 63 (tadalafil) mg/one dose.