• Journal of the Korean Chemical Society
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• v.59 no.3
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• pp.225-232
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• 2015

A liquid chromatography-electrospray ionization-tandem mass spectrometry method (LC-ESI-MS/MS) was used for determining seven pesticides (2,4-dichlorophenoxyacetic acid, methomyl, aldicarb, 2-methyl- 4-chlorophenoxy- acetic acid, molinate, carbaryl and carbofuran) and two synthetic materials (quinoline and bisphenol-A) in surface water. The analytes were extracted using solid-phase extraction (SPE). The eluate was concentrated by nitrogen gas. 100 microliters of 30% (v/v) methanol aqueous solution were used to dissolve the residue and an aliquot of the reconstituted solution was directly injected into LC-ESI-MS/MS after the filtration using 0.2 μm polytetrafluoroethylene (PTFE) syringe filter. Under the established condition, the calibration curves of the analytes were linear with correlation coefficients of above 0.997. The quantification limit was 0.002~0.011 μg/L and the relative standard deviations were less than 16.4%. In addition, accuracy was in the range of 84~107% and the recoveries were values between 56.2 and 98.6%. In this study, the developed method was applied to the analysis of real surface water samples.

• Korean Journal of Environmental Agriculture
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• v.18 no.2
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• pp.135-139
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• 1999

A new effective and economic method was developed, removing interferences such as chlorophyll and lipid from leaves with small amounts of reagents and solvents in order to analyse PAHs(Polycyclic Aromatic Hydrocarbons). The extract from a soxhlet containing $4{\sim}5g$ of leaves and 100ml of dichlormethane and refluxed for 20 hrs was concentrated and eluted with 60ml of a hexane:dichloromethane (1:1) mixture through a column of 9mm wide inner diameter and 130mm long, packed from the bottom with 2.5g of $Al_2O_3$, 1.5g of $SiO_2$and 2g of anhydrous $Na_2SO_4$. The eluent was concentrated and loaded on a GPC column of 20mm wide inner diameter and 280mm long, packed with 12g of Bio-beads. The column was washed with 37ml of the hexane:dichloromethane(1:1) mixture. Another 43ml of the mixture was eluted as a PAH fraction and collected. This eluent was concentrated under gentle nitrogen to $50{\mu}l$ and analysed using GC-MS. The recoveries, obtained by comparing with the amounts of the internal standards of deuterated PAHs were $43.3{\sim}107.5%$(RSD $2.2{\sim}9.5%$).

• Korean Journal of Soil Science and Fertilizer
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• v.25 no.4
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• pp.387-393
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• 1992

The fate of inoculum strain of Bradyrhizobium japonicum was studied by using genetically marked strain. RJB6 $str^rnal^rneo^r$. A spontaneous mutant of B. japonicum isolated from nodules was made to have antibiotic resistance against streptomycin and nalidixic acid. In order to make genetically marked strain, neomycine resistant gene(Tn5) was introduced into this spontaneous mutant by conjugation with E. coli containing pSUP2021. The southern hybridization was carried out to confirm the plasmid insertion. Hybridization of chromosome DNA using pSUP2021(Tn5) as a probe showed that Tn5 was located on the 4.9kb fragment of chromosome. Soybean seeds were planted into a soil previously cultivated with soybean and inoculated with different cell densities of marked strain. Fourty days after planting, the inoculation effects on nodule number, nodule fresh weight, plant height and nitrogen content in the plot inoculated with heavy cell suspension was a little better than those in the plot with low inoculation. The recovery percentage of the marked strains was about 12% in the plot inoculated with heavy density cell suspension, while 5% in the plot inoculated with low cell suspension.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.30 no.5
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• pp.753-758
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• 1997

Dried alaska pollack is one of the representatives among dried marine fish and shellfish products in our country. This study was performed to obtain the basic data about the effect of drying method on the formation of N-nitrosamine and its precursor to ensure the safety of dried alaska pollack. The contents of nitrate and nitrite were detected 1.5 and <1.0 mg/kg in raw samples, and $3.0\~4.2,\;1.4\~2.7mg/kg$ in dried products, respectively. There was no significant change of betaine contents during drying while TMAO decreased, TMA and DMA increased in alaska pollack during d교ing. N-nitrosodimethylamine (NDMA) was only detected in alaska pollack and its dried products, and recovery from above samples spiked with $10{\mu}/kg$ for N-nitrosodipropylamine was $87.2\~107.4\%$. The levels of NDMA were found to be $2.8{\mu}/kg$ on an average in raw samples, but the levels of NDMA increased remarkably during drying of alaska pollack and its content in dried products was $8.7\~51.4{\mu}g/kg$. Regardless of drying methods, NDMA tend to increased in dried products, and its contents were 15.5 times higher in hot-air dried than raw samples, 9.0 times in sun dried and 4.4 times in freeze dried products. less NDMA was produced in the freeze dried products, so it is believed that freeze drying method is effective to decrease the NDMA levels in the dried products of alaska pollack.

• Journal of the Korean Chemical Society
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• v.38 no.9
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• pp.667-675
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• 1994

The precipitate flotation using $La(OH)_3$ as a coprecipitant was studied for the simultaneous determination of trace three elements in a sea water. Several experimental conditions such as pH, coprecipitant and surfactant were investigated with an artificial sea water. To remove the influence of Cr(VI) the Cr(VI) was reduced to Cr(III) using $NaBH_4$ prior to the flotation. Trace amounts of Cu(II), Co(II) and total Cr in 1.0 l sea water was coprecipitated together with the precipitation of $La(OH)_3$ in the solution of pH 9.8 adjusted with 3.OM NaOH solution. The precipitate was floated by using a mixed surfactant (1 to 8 of each 0.5% ethanolic sodium oleate and sodium dodecylsulfate solution) by bubbling a nitrogen gas. The floats was separated and filtrated from the mother liquor by suction. The precipitate was dissolved in 7.0 M $HNO_3$ solution and then marked to 25.0 ml with a deionized water. These elements were determined by graphite fumace atomic absorption spectrophotometry. This method was applied to determine the elements in the sea water of the Eastern and Western coasts. And the recoveries were over 90.0% in the samples into which given amounts of the analyte elements were spiked.

• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.389-396
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• 1991

The pre-concentration and determination of ultratrace arsenic in water samples was studied by the precipitate flotation technique. The arsenic in 1.0l of water sample, in which all suspended materials were filtered out, was coprecipitated together with La(OH)$_3$ precipitates at pH 8.5${\pm}$0.1. After the precipitate was made to be hydrophobic by adding mixed surfactant of 1 : 8 mole ratio of sodium oleate and sodium dodecyl sulfate, it was floated with the aid of tiny bubbles of nitrogen gas in a flotation cell. The floated precipitate was quantitatively collected on a micropore glass filter by the suction, dissolved with small volume of 1.0M sulfuric acid, and accurately diluted to 25.00ml with a de-ionized water. Total arsenic was spectrophotometrically determinated by forming silver diethyldithiocarbamate complex of arsine generated from arsenic in the concentrated solution. The calibration curve was linear up to 20ng/ml in the original solution. Analytical results showed that contents of arsenic in a campus wastewater and a river water were 8.2ng/ml and l.0ng/ml, respectively, and their recoveries were 93${\%}$ and 90${\%}$ in water samples which a given amount of arsenic was added into. From above result, it could be concluded that this method was applicable to the determination of arsenic in various kinds of water at low ng/ml levels.

• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.355-361
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• 1991

The separative preconcentration of trace mercury[Hg(II)] in a water sample was studied by a coprecipitation flotation technique. The trace Hg(II) was precipitated together with Ce(OH)$_3$ by adding 3.0 ml of 0.1M Ce$^{3+}$ solution to 1,000 ml of water sample and adjusting pH to 11.0 with 1.0M NaOH solution. The hydrophobic precipitate[Ce(OH)$_3$-Hg(OH)$_2$], which was formed by adding 2.0 ml of 0.1${\%}$ ethanolic sodium oleate solution, were floated on the surface with an aid of tiny nitrogen gas bubbles. The floated materials were quatitatively collected in a suction flask and dissolved with 5.0 ml of 2.0M HNO$_3$. The solution was marked to 25.00 ml with a deionized water. The content of Hg(II) was determined by cold vapor atomic absorption spectrophotometry. Any interferences of concomitants such as Ag$^+$, Br$^-$, I$^- $, etc. were not observed on the whole procedure. The analytical result showed that Hg(II) found in the wastewater of Seochang Campus, Korea University was 1.98 ng/ml with the relative standard deviation of 3.6${\%}$. And recoveries of Hg(II) in the wastewater into which 1.0 ng/ml and 2.0 ng/ml were added were 95${\%}$ and 91${\%}$, respectively. From such results, this procedure could be concluded to be tolerably accurate and reproducible for the determination of trace mercury in a water sample.

• Journal of the Korean Chemical Society
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• v.40 no.12
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• pp.724-732
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• 1996

The organic precipitate flotation using Cu(II)-pyrrolidinedithiocarbamate complex as a coprecipitant was studied for the preconcentration and determination of trace Cd, Pb, Bi and Co in several water samples. Experimental conditions such as pH of solution, amounts of Cu(II) and ammonium pyrrolidinedithiocarbamate(APDC), stirring time, the type and amount of surfactant, etc. were optimized for the effective flotation of analytes. After 3.0 mL of 1,000 ${\mu}g/mL$ Cu(II) solution was added to 1.00 L water sample, the pH of the solution was adjusted to 2.5 with HNO3 solution. Trace amounts of analytes were coprecipitated by adding 2.0% APDC solution. And the precipitates were flotated onto the surface of solution with the aid of nitrogen gas and sodium lauryl sulfate. The floats were collected from mother liquor, and filtered through the micropore glass filter by suction. The precipitates were dissolved with 4 mL conc. HNO3, and then diluted to 25.00 mL with deionized water. The analytes were determined by graphite furnace atomic absorption spectrophotometry. This flotation technique was applied to the analysis of some water samples, and the 90 to 120% of recoveries were obtained from the spiked samples, this procedure could be concluded to be simple and applicable for the trace element analysis in various kinds of water.

• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.327-333
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• 1993

A method was developed for the determination of trace elements in seawater by precipitate flotation preconcentration and subsequent flame atomic absorption detection. In order to quantitatively coprecipitate trace ions such as Cd(II), CuI(II), Fe(III), Mn(II), Pb(II) and Pd(II), 2.0 ml of 1.0M cerium(III) solution was added to 1.0l of seawater and the pH was adjusted to 9.5 with 5.0 M sodium hydroxide solution while stirring with a magnetic stirrer. The precipitate was floated with the aid of surfactant solution (1.0 ml of 0.3% sodium oleate) by bubbling nitrogen gas through a porous (No. 4) fritted glass disk. The floats was collected in a small Erlenmeyer flask by suction. The washed precipitate was dissolved in 8.0 M nitric acid and marked with deionized water in the volumetric flask of 10.0 ml. The analyte was determined by measuring the atomic absorbances in 100-fold concentrated solution. Above all analytes in Kangnung (East Sea) and Kanghwado (West Sea) sea waters were found to be under the detection limit of this method. The recoveries of over 92% for all analytes spiked into seawater samples showed that this method was applicable to the analysis of real seawater.

• Korean Journal of Plant Resources
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• v.34 no.4
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• pp.384-394
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• 2021

The aim of this study was to investigate the correlation between soil properties and marker compounds contents of Paeonia lactiflora. The methods of determining marker compounds were validated by measuring the linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy and recovery using UPLC analysis. P. lactiflora contained albiflorin at 0.04 ± 0.00 ~ 2.79 ± 0.21%, paeoniflorin at 1.98 ± 0.14 ~ 6.67 ± 0.84%. The root dry weight (RDW) of P. lactiflora was 0.06 ± 0.02 ~ 1.27 ± 0.28 kg. The soil properties analysis such as soil pH, electric conductivity (EC), organic matter (OM), total nitrogen (TN), available phosphate (Avail. P₂O₅), exchangeable cation and cation exchange capacity (CEC) were performed following standard analysis manual. The results of correlation analysis between soil properties and growth characteristics, available P₂O₅ was positively coreelated with the RDW of P. lactiflora. On the other hand, the RDW of P. lactiflora showed significantly negative correlation with contents of albiflorin and paeoniflorin. The results of this study was might be help to provide useful information on the establish of standard cultivation by the investigate correlation analysis between growth characteristics and marker compound contents of P. lactiflora.