• Journal of the Korean Chemical Society
• /
• v.33 no.1
• /
• pp.70-81
• /
• 1989

Reverse phase liquid chromatographic elution behaviors of salicylic acid and its derivatives were studied with classical and modern high-performance liquid chromatography(HPLC) using Amberlite XAD-4 and XAD-7 resin packed columns. Capacity factors(k') were determined in the comparatively high concentration(from 0. 010F to 0. 150F) of ferric nitrate-50% methanol solution to elucidate the elution behaviors with classical method. On the other hand, k's were measured in the various concentrations of methanol and ferric nitrate(from $2.5{\times}10^{-4}F\;to\;1.0{\times}10^{-3}F$) solution of pH 2. 25 and 293K with HPLC to explain the elution mechanism of them, and to find their optimum separation condition. As a result, it was found that log k's of salicylic acid and its derivatives were decreased with increasing the concentration of ferric ion, and the decreasing slopes of the compounds on the increasing ferric ion concentrations were related with each stability constant of ferric salicylates. Some isomers of derivatives of salicylic acid could be separated in the optimum condition.

• Analytical Science and Technology
• /
• v.16 no.2
• /
• pp.102-109
• /
• 2003

Microwave digestion and solid-state extraction were studied for determination of trace aluminum{Al(III)} in human urine samples. A mixed acid of nitric acid and hydrogen peroxide was added to urine samples, organic materials were destructed in a home microwave oven and dried in a drying oven. The dried residues were dissolved in a sulfuric acid solution. The solution was eluted through a XAD-4 resin column adsorbed with 8-hydroxyquinoline(Oxine, HQ). Al(III)-8-hydroxyquinolinate complex was formed in the column and eluted with 0.5 M nitric acid solution. The Al(III) eluted was determined by graphite atomic absorption spectrophotometry. Various experimental conditions of followings were investigated for the optimization : the type of acid to dissolve the residues, the amount of HQ adsorbed on the resin, the pH of sample solutions, the type and concentration of acid to elute the complex from column and so on. The contents of Al(III) in real samples were determinated by a calibration curve method. The recovery in standard spiked samples was 94~101% and the detection limit of this procedure was 0.05 ng/mL.

• Korean Journal of Weed Science
• /
• v.12 no.1
• /
• pp.52-60
• /
• 1992

There was no significant difference in the final germination percentages(Experiment 1-3) as affected by sunflower root exudates between the control and the treated for the test species. In general(Experiment 1), however, germination onset was delayed the treated bottles. Germination rate was, also, reduced for both radish(Raphanus sativus L.) and rice(Oryza sativa L.). Therefore, the germination index was low in the treated bottles but germination gradually increased with time in the greated bottles in all test species so that the final germination percentages were similar between treatments. The root exudates of sunflower had significant inhibitory effects(Experiment 1-3) on the lengths of the shoots and roots of all the test species. Fresh weight was also significantly reduced in all test species. Sunflower seedlings(Experiment 3) in the treated(with the XAD-4 resin column) were larger and healthier than those in the control (without XAD-4 resin column) because of the removal of allelochemicals. The fresh weight of sunflower seedlings was markedly inhibited by sunflower root exudates. These mean that sunflower probably is an autotoxic crop.

• Journal of Microbiology and Biotechnology
• /
• v.8 no.5
• /
• pp.478-483
• /
• 1998

For the enhanced production of a cardiac glycoside, digoxin, using in situ adsorption by biotransformation from digitoxin in plant cell suspension cultures, selection of proper resins was attempted and the culture conditions were optimized. Among various kinds of resins tested, Amberlite XAD-8 was found to be the best for digoxin production in considering adsorption characteristics as well as the effect on cell growth. Adequate time for resin addition was determined to be 36 h from the beginning of biotransformation and the presence of resins should be as short as possible to increase the productivity. In addition, to prevent the cells from direct contact with resin particles, immobilized systems were designed and examined. Immobilization further improved the advantages of in situ adsorption. It was confirmed that the increase of the contact area for mass transfer was an important factor in utilizing an immobilized system to enhance digoxin production.

• Proceedings of the Korea Society of Environmental Toocicology Conference
• /
• 2002.10a
• /
• pp.163-163
• /
• 2002

국내에서 사용중인 농약에 대한 농민의 농약 노출량 및 양상을 조사하고자 내분비계 장애 물질로 추정되는 Mancozeb의 살포 시 작업자의 피부 노출량 및 호흡 노출량 측정을 감귤농장에서 실시하였다. 피부노출 측정은 Patch법(50$\textrm{cm}^2$)을 사용하였고 손 노출은 순면장갑을 사용하였다. 호흡노출은 XAD-2 resin 흡착제와 Personal air monitor(2L/min)를 이용, 측정하였다. Mancozeb 분석은 CS$_2$법을 이용하였고 patch, resin, 장갑, 마스크, 소변에서 Mancozeb의 회수율 및 포장회수율 모두 90%이상이었다. 감귤 재배시 Mancozeb 사용에 따른 피부노출량은 여자가 약 1800mg/hr, 남자는 약 1300mg/hr 이었고 주로 배, 등, 상박 그리고 허벅지에 노출량이 많았다. 호흡노출은 관찰되지 않았고 소변에서도 Mancozeb는 관찰되지 않았다. 위해성 평가를 위해 PDE, AQE 및 MOS를 구하였으며 MOS는 Severn의 공식을 이용하였다. MOS는 여자가 0.37, 남자가 0.58이었다.

• Asian Journal of Turfgrass Science
• /
• v.10 no.3
• /
• pp.263-270
• /
• 1996

This experiment was conducted to investigate the loss of various herbicides by means of vola-tility from the turfgrass field and the hare ground with the different soil moisture contents and temperatures. Different herbicides were applied at the rates of 375 g a.i. /l0a of pendimethalin,250 g a.i. /l0a of napropamide, and 96.4 g a.i. /l0a of dicamba with 200 \ulcorner/10a of spray volume in the turfgrass(Zoysia japonica cut off 5cm) grown in pots(265.8 $cm^2$) and bared soil. The pots were placed in the growth chamber with 10,000 lux of light intensity(12h per day) at 25 and 35˚C for 7days. Amberlite XAD polymeric resin(20/50 mesh) was used as sampling media for herbicide airborne residues. Air flow was maintained at 10 \ulcorner /min by vacuum pump regulated with a factory calibrated flow meter. Herbicide airborne residues were extracted from the XAD resin with 300 ml of 1:1 acetone and hexane. The extracts were concentrated by rotary evaporation at 35˚C and dissolved in 1 ml MeCN for HPLC analysis. The airborne losses of the herbicide applied in the turfgrass and bare soil increased as the temperature and soil moisture contents were increased, regardless of the kinds of herbicide. Higher airborne residues was observed in the turfgrass pots than the bare soil pots. Pendimethalin and dicamba with higher vapor pressure gave rise to the increased loss of airborne herbicides, showing that 6.26 and 6.4% of average airborne loss in pendimethalin and dicamba, respectively, compared to 0.56% in napropamide. The amount of airborne losses in turfgrass was highest at one day after application and then a declined trend was observed as the time was prolonged. Key words. Herbicides, Turfgrass field, Bare ground, Volatility.

• YAKHAK HOEJI
• /
• v.44 no.5
• /
• pp.384-390
• /
• 2000

Metabolism study of the dye, benzidine, was performed by gas chromatography-mass selective detector (GC/MSD) in the urine of rats orally administered 100 mg/kg benzidine. Urine samples were collected in metabolic cages for 0-24, 24-48, and 48-72 hrs. Ten ml of the urine was extracted with XAD-2 resin and the XAD-2 column was eluted with methanol. After evaporation, benzidine and its metabolites were extracted with diethyl ether (for non-conjugated fraction). For conjugated metabolites, $\beta$-glucu-ronidase was added to the aqueous layer that was incubated for 1 hr at 5$0^{\circ}C$ and the aqueous layer was extracted as in non-conjugated fraction. Aliquot of trimethylsilylated derivatives was applied to the GC/MSD. The mutagenicity of benzidine and its acetylated metabolites was tested by histidine/reversion assay. Five metabolites observed and confirmed either by electron impact and chemical ionization modes of the GC/MSD, or authentic compounds were monoacetyl-, diacetyl-, hydroxyacetyl-, hydroxydiacetyl-, and hydroxy-benzidine. Monoacetyl-benzidine was more potent than benzidine in histidine/reversion assay. This data indicates that monoacetylation of benzidine may be one of the metabolites produced in metabolic activation process.

• Journal of Industrial and Engineering Chemistry
• /
• v.67
• /
• pp.461-468
• /
• 2018

A highly sensitive, selective and rapid method for the determination of lead based on the reaction of lead (II) with 5-(4'-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione (CPAHPD) and the solid phase extraction of the Pb(II)-CPAHPD complex with Amberlite XAD-2000 was developed, in the presence of pH 5.6 buffer solution and Triton X-114 medium. CPAHPD reacts with lead to form a violet complex with a molar ratio of 2:1 (CPAHPD to lead). This complex was enriched by the solid phase extraction with Amberlite XAD-2000. An enrichment factor of 500 was obtained by elution of the complex from the resin with a minimal amount of isopentyl alcohol(0.2 mL). In isopentyl alcohol medium,the molar absorptivity of the complex is $1.13{\times}10^6L\;mol^{-1}cm^{-1}$ at 647 nm. Beer's law is obeyed in the range of $5.0-160ng\;mL^{-1}$ in the measured solution. The relative standard deviation for 10 replicate samples of $50ng\;mL^{-1}$ level is 1.26%. The detection and quantification limits reaches 1.5 and $4.7ng\;mL^{-1}$ in the original samples. The presented procedure was successfully applied for determination of lead content in real samples such as vegetables, waters, biological and soil samples with satisfactory results.

• The Korean Journal of Pesticide Science
• /
• v.19 no.3
• /
• pp.230-240
• /
• 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
• /
• v.9 no.4
• /
• pp.364-372
• /
• 1996

The sorption and desorption properties of U(VI), Th(IV), Zr(IV), Cu(II), Pb(II), Ni(II), Zn(II), Cd(II) and Mn(II) ions on XAD-16-[2-(2-thiazolylazo)-p-cresol](TAC) chelating resin were studied by elution method for selective separation, concentration and recovery of trace metal ions in sea water. The optimum conditions for the sorption of metal ions were examined with respect to flow rate, pH and concentration of buffer solution. The overall capacities of some metal ions on this chelating resin were 0.41mmol U(VI)/g resin, 0.55mmol Th(IV)/g resin, 0.43mmol Cu(II)/g resin, and 0.32mmol Zr(IV)/g resin, respectively. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 5.0 was found as Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Cd(II)>Mn(II). Desorption of characteristics for metal ions were investigated with desorption agents such as $HNO_3$, HCl, $HClO_4$, $H_2SO_4$, and $Na_2CO_3$. It was found that most of metal ions except Zr(IV) showed high desorption efficiency with 2M $HNO_3$. But, desorption and recovery of Zr(IV) ion were successfully performed with 1M $H_2SO_4$. The resin was applied for separation and preconcentration of trace amount of U(VI) ion from artificial sea water and the recovery of U(IV) was over 96%.