• Analytical Science and Technology
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• v.20 no.4
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• pp.347-354
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• 2007

A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in bovine, porcine, chicken, flatfish and japanese eel muscle has been developed and validated. The separation condition for HPLC/UV was optimized with phenyl hexyl ($4.6{\times}150mm$, $5{\mu}m$) column with 10 mM monobasic sodium phosphate buffer (pH 2.5)/acetonitrile (50/50, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection wavelength was set at 254 nm. Residues were extracted from tissue by blending with methanol and lipid materials were removed with n-hexane. Then, the methanol extract was evaporated to dryness under a nitrogen stream, reconstituted in the mobile phase. Aliquot of the organic extract was decanted and filtered through $0.45{\mu}m$ syringe filter. The $20{\mu}L$ of the resulting solution was injected into the HPLC system. The calibration ranges were $0.5{\sim}5{\mu}g/g$ and calibration curves were linear with coefficients of correlation better than 0.95. The limits of quantification were $0.5{\mu}g/g$ for all muscles. The recoveries of bovine, porcine, chicken, flatfish and japaneseel muscles were 99.8%, 102.4%, 91.0%, 104.0% and 93.0%, respectively. The procedures were validated according to the CODEX guideline, determining specificity, linearity, accuracy, precision, quantitation limit and recovery.

• Analytical Science and Technology
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• v.20 no.5
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• pp.393-399
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• 2007

In principle, the blood galactose level may be determined conveniently with a strip-type biosensor similar to that for glucose. In this study, we describe the development of a disposable galactose biosensor strip for point-of-care testing. The sensor strip is constructed with screen-printed carbon paste electrode (SPCE) and sample amount (< $100{\mu}L$). The developed strip the galactose level in less than 90 s using bienzymatic system of galactose oxidase (GAO) and horseradish peroxidase (HRP). The effects of pH, mediator (1,1-ferrocenedimethanol) concentration, ratio of enzymes, and applied potential were determined preliminarily with glassy carbon electrodes, and optimized further with the strip-type electrodes. The sensor exhibits linear response in the range of $0{\sim}400{\mu}M$ ($r^2$ = 0.997, S/N = 3). Since a low working potential, in principle, the fabricated disposable galactose biosensor has -100 mV (vs. Ag/AgCl), it is applied for the detection of galactose, interfering responses from common interferents such as ascorbic acid, uric acid and acetaminophen could be minimized. The sensor has been used to determine the total galactose level in standard samples with satisfactory reproducibility (CV = 5 %).

• Analytical Science and Technology
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• v.21 no.5
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• pp.412-423
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• 2008

A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

• Analytical Science and Technology
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• v.21 no.3
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• pp.212-221
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• 2008

In order to investigate the information for effective detection and developing of latent fingerprints, we identified fatty acids composition of latent fingerprints on non-porous evidence surface and the chemical changes of latent fingerprint residue after print deposition during 7 months. Fingerprints from eight Korean male donors (aged 29-50 years) and one female donor (aged 36 years) were collected. All fingerprints were found to contain lauric acid (C12:0), myristic acid (C14:0), palmitic acid (C16:0), stearic acid (C18:0), elaidic acid (C18:1n9t), oleic acid (C18:1n9c), linoleic acid (C18:2n6c), arachidic acid (C20:0), linolenic acid (C18:3n3), erucic acid (C22:1n9) and docosadienoic acid (C22:2) and primarily palmitic acid (35.45-48.37%), oleic acid (14.84-28.49%), stearic acid (9.71-24.96%) and linoleic acid (7.68-18.8%) occupied 75% of total fatty acids. When the fingerprints were deposited at dark room for 7 months, total fatty acids components decreased about 12-25%. It can be explained that significant degradation of long-chain fatty acids such as elaidic acid (C18:1n9t), arachidic acid (C20:0), linolenic acid (C18:3n3), erucic acid (C22:1n9), and docosadienoic acid (C22:2) resulted in the generation of myristic acid (C14:0), myristoleic acid (C14:1) and pentadecanoic acid (C15:0).

• Analytical Science and Technology
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• v.22 no.3
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• pp.191-200
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• 2009

The aim of this study was to evaluate and establish of emission test method for liquid phase building materials such as paint, adhesive, sealant by emission cell. A small-scale emission chamber and emission cell were used to evaluate emission of TVOC from paint, adhesive, sealant. The quantity of TVOC emission were measured by a gas chromatography/mass spectrometry (GC/MS). Background concentration of TVOC was below $10{\mu}g/m^3$ in the emission chamber and cell. Air tightness and recovery in chamber and cell showed good results. The recovery of thermal desorber for toluene and n-dodecane were about 120%. The repeatability of response factor and retention time in GC/MS below 30%. The method detection limit of VOCs ranged 0.04~8.82 ng. The concentration of TVOC emission using emission cell was 1.35~1.41 times higher than emission chamber. The correlation of TVOC emission using chamber and cell method was significantly high (r=0.91~0.97).

• Analytical Science and Technology
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• v.22 no.1
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• pp.44-50
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• 2009

In this study, the use of purge & trap GC-MS technique for determination of methylmercury in sediment samples was described. The method detection limit of the method was determined as 0.06 ng/g and the recovery of the method was $102{\pm}11.4%$, with precisions better than 11.2%. The method was validated by analysis of CRMs such as ERM CC580 (estuarine sediment) and IAEA 405 (sediment). Additionally, the performance of the method was tested on river sediment samples and the analytical results were compared with those of the GC-CVAFS, which has been widely used for methylmercury analysis.

• Analytical Science and Technology
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• v.22 no.3
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• pp.272-276
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• 2009

This study was performed to investigate the disinfection efficiency and the generation characteristics of disinfection by-products (DBPs) in the sewage effluent. In the case of total coliforms, disinfection efficiency higher than 99%, the required contact time was 30 min at chlorine dose of 0.5 mg/L, 20 min at 1.0 mg/L, and 10 min at 1.5 mg/L, respectively. When the sewage effluent was disinfected with chlorine dose of 0.5 mg/L for 10 min, the maximum generation concentration of trihalomethanes (THMs), haloacetonitriles (HANs) and haloacetic acid (HAAs) were $32.2{\mu}g/L$, $2.97{\mu}g/L$, and $16.29{\mu}g/L$, respectively. The concentration of chloroform was $28.4{\mu}g/L$ corresponding to 88.1% of the THMs. The concentration of HANs and HAAs were found to be inconsiderable. The average residual chlorine concentration of sewage effluent was 0.4 mg/L, the generation concentration of THMs was maximum $1.72{\mu}g/L$ and average $2.79{\mu}g/L$. HANs and HAAs were under the detection limit by GC/MSD.

• Analytical Science and Technology
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• v.22 no.3
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• pp.235-246
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• 2009

The analyses of minor and trace elements in glass debris were performed using LA-ICP-MS in order to identify manufacturers using real commercial samples. At first, a calibration curve was made using standard glass samples of NIST 610, 612, 614 and 616. $^{29}Si$ was used as an internal standard, and the ratios of metal/Si for each metal were compared with their concentrations. Based on elements in each sample and standard materials, 24 metals were quantified and the LOD in analysis, according to the blank sample, was in the range of 0.11 mg/kg (Ti)-4.91 mg/kg (Ca). Eleven samples from two manufacturers were collected and five sub-samples were taken from each sample for analysis. 15 elements (Co, Ce, Ca, Mn, Sr, Ba, Li, Rb, U, La, Th, Na, Al, Zr and Hf) were selected to identify manufacturers because some elements (Cu, Cr, Cd and Ni) were below the detection limit and some elements (Ti, Pr, Mg, Nb, Nd) were absent in the analysis of standards and others (Pb and Sn) had a problem of homogeneity. The attempts to identify manufacturers and the manufacturing period were performed through a triangular diagram. In the manufacturer discrimination by discriminant analysis, a canonical discriminant function was made based on Mn, Ce and Rb, and each sample could be identified.

• 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.22 no.4
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• pp.345-353
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• 2009

The new anti-impotency analogue was identified in food source. Detection of this analogue was accomplished through screening of food samples by liquid chromatography/photodiode array detector. The spectrum pattern of analogue compound was similar to that observed for hongdenafil which was analogue of sildenafil. This new compound was isolated and purified using the liquid-liquid extraction, thin layer chromatography, column chromatography and preparative HPLC. And then those structure were identified using analytical instruments such as HPLC/PDA, LC/MS/MS and NMR. The compound was given a name to oxohongdenafil which was replaced with acetyl oxoethylpiperazinyl residue instead of sulfonyl piperazine group of sildenafil. The regulation for the abovementioned analogue, oxohongdenafil, was established by Standard of Korean food code.