• Korean Chemical Engineering Research
• /
• v.47 no.2
• /
• pp.258-261
• /
• 2009

In this work, we the ettect on extraction amounts and general composition content of phytoestrogen genistein and formononetin extracted from Sophoraflavescens Aiton by various ultrasonic waves(35, 72, and 170 KHz) and extraction time(30, and 60 min) were compared using extraction solvent water 100%. The pretreatment step was composed of ultrasonic waves extraction, filtration, concentration, and membrane filtration. The extracted sample was analyzed by reversed-phase high performance liquid chromatography(RP-HPLC). And the mobile phase applied was linearly changed with A/B of 80/20~65/35 vol% for 60 min(A water/acetic acid, 99.9/0.1 vol%, B acetonitrile/acetic acid, 99.9/0.1 vol%). The experimental results, general composition carbohydrate(0.255 to 0.413%) excepts, other ingredients was confirmed almost similarly. Also, The highest yield of extraction amount 3.17g was obtained by ultrasonic waves with a frequency of 170 KHz and an extraction time of 60 min. This work offers would be useful for chemical and biological studies of natural plants and its products.

• Analytical Science and Technology
• /
• v.26 no.5
• /
• pp.307-314
• /
• 2013

Selenium exists in various forms of chemical species. The activity and bioavailability is strongly dependent on its chemical form and concentration. Consequently the information on each selenium species and its concentration must be exactly determined for the food we take in. In this study, selenium species in seafood were separated and quantified by RP (reversed phase) HPLC (high performance liquid chromatography) coupled with ICP-MS (inductively coupled plasma mass spectrometry) using post-column isotope dilution. $^{79}Br$, which interferes on $^{80}Se$, has mostly been removed by solid phase extraction and then mathematical correction has been applied for the more accurate correction. The experimental result for CRM (certified reference material) DOLT-4 agreed well with the certified value but each selenium species could not be compared. SeCys (selenocysteine) and SeMet (selenomethionine) were the major species detected in seafood such as belt fish, spanish mackerel, and squid that have been serving as Korean diet. The concentrations found in Korean sea food for SeCys and SeMet were in the range of 0-661.6 mg/kg and 137.3-462.7 mg/kg, respectively.

• Resources Recycling
• /
• v.29 no.2
• /
• pp.69-77
• /
• 2020

With rapid increasing production and installation, recycling of photovoltaic modules has become the main issue. According to the research, the accumulation of waste modules will reach to 8600 tons in 2030. Moreover, Crystalline-silicon (c-Si) Photovoltaic modules account for more than 90% of the waste. C-Si PV modules contain 1.3% of weight of photovoltaic ribbon inside which contains the most of lead, tin and copper in the PV modules, which would cause environmental and humility problem. This study provided a valuable metal separation process for PV ribbons. Ribbons content 82.1% of Cu, 8.9% of Sn, 5.2% of Pb, and 3.1% of Ag. All of them were leached by 3M of hydrochloric acid in the optimal condition. Ag was halogenated to AgCl and precipitated. Cu ion was extracted and separated from Pb and Sn by Lix984N then stripped by 3M H2SO4. The effect of the optimal parameters of extraction was also studied in this essay. The maximum extraction efficiency of Cu ion was 99.64%. The separation condition of Pb and Sn were obtained by adjusting the pH value to 4 thought ammonia to precipitate and separate Pb and Sn. The recovery of Pb and Sn can reach 99%.

• Analytical Science and Technology
• /
• v.21 no.4
• /
• pp.259-271
• /
• 2008

The analytical method of extracting compounds from human blood to examine accumulated organochlorine pesticides (OCPs) has been widely used the traditional liquid-liquid extraction (LLE) method and solid-phase extraction (SPE) method, yet these methods have certain limitations in purification and usafe of a large amount of sample. In order to overcome the se problems reside in these, solid-phase microextraction (SPME), known as a highly efficient extration method with less samples and relatively simple, was employed to collect 18 different kinds of OCPs in blood as extraction method in this study. To optimize extraction method, we examine various experimental SPME-parameters such as adsorption (fiber type, adsorption time, adsorption temperature, salting out effect), and desorption (desorption time, desorption temperature etc.). From the experimental results, the optimal conditions are as follows: fiber was polyacrylate with $85{\mu}m$, adsorption time was for 5 min, adsorption optimum temperature was at $280^{\circ}C$, and salting out effect was NaCl with 0.1 g. MDL, precision and accuracy was in the ranges of 0.05~0.20 ng/mL, 5.59~13.39%, respedively, and accuracy was -0.5% ~24.5% for all OCPs.

• Bulletin of the Korean Chemical Society
• /
• v.31 no.5
• /
• pp.1192-1198
• /
• 2010

Pharmaceuticals and personal care products (PPCPs) are emerging contaminants in the aquatic environment. Many pharmaceuticals are not completely removed during wastewater treatment, leading to their presence in wastewater treatment effluents, rivers, lakes, and ground water. Here, we developed analytical methods for monitoring ten pharmaceuticals from surface water by LC/ESI-MS/MS. For sample clean-up and extraction, MCX (mixed cation exchange) and HLB (hydrophilic-lipophilic balance) solid-phase extraction (SPE) cartridges were used. The limits of detection (LOD) in distilled water and the blank surface water were in the range of 0.006 - 0.65 and 1.66 - 45.05 pg/mL, respectively. The limits of quantitation (LOQ) for the distilled water and the blank surface water were in the range of 0.02 - 2.17 and 5.52 - 150.15 pg/mL, respectively. The absolute recoveries for fortified water samples were between 62.1% and 125.4%. Intra-day precision and accuracy for the blank surface water were 2.9% - 24.1% (R.S.D.) and -16.3% - 16.3% (bias), respectively. In surface wastewater near rivers, chlortetracycline and acetylsalicylic acid were detected frequently in the range of 0.017 - 5.404 and 0.029 - 0.269 ng/mL, respectively. Surface water near rivers had higher levels than surface water of domestic treatment plants.

• Bulletin of the Korean Chemical Society
• /
• v.29 no.6
• /
• pp.1173-1178
• /
• 2008

A simple and sensitive high-performance liquid chromatographic method was developed for the simultaneous identification of enrofloxacin and its active metabolite ciprofloxacin in chicken muscle. Norflorxacin imprinted polymers synthesized in water-containing systems show high selectivity to enrofloxacin and ciprofloxacin in an aqueous environment. Using these water-compatible imprinted polymers as selective adsorbents in the solid-phase extraction of enrofloxacin and ciprofloxacin from chicken samples, the remaining biological matrix could be quickly washed out from the imprinted column while enrofloxacin and ciprofloxacin were selectively retained and enriched. Analytical separation was performed on a $C_{18}$ column using acetonitrile-water as a mobile phase and fluorescence detection. Good linearity was obtained from 0.8 to 500 ng/g (r > 0.998) with relative standard deviation of less than 3.9%. The mean recoveries of enrofloxacin and ciprofloxacin from chicken muscle were 80.6-94.5% and 77.8-91.8% at three different concentrations. The limits of determinations based on S/N=3 were 0.07 ng/g and 0.09 ng/g, which are below the maximum residue limits established in many countries.

• Analytical Science and Technology
• /
• v.28 no.6
• /
• pp.370-376
• /
• 2015

An analytical method for determining phenol considered priority pollutants of the US EPA and precursor of toxic phenolic compounds by solid-phase extraction (SPE) and high performance liquid chromatographic systems (HPLC) equipped with fluorescence and mass selective detectors have been developed. The SPE process for sample preconcentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of pH, elution solvent, and elution volume on the recoveries of the analytes were investigated with HPLC/FLD. Average recovery of >87.0% was achieved with 60 mg sorbents using 5 mL of methanol as an elution solvent at pH=3.

• Journal of Soil and Groundwater Environment
• /
• v.15 no.4
• /
• pp.13-20
• /
• 2010

The purpose of this study was to develope the remediation method of contaminated soils with metals and petroleum. The diesel degrading strain was isolated and identified from the soil contaminated by petroleum at industrial sites. Diesel biodegradation experiment was performed by diesel degrading bacteria in both solution and soil slurry. Contaminated soils by Zn or As and diesel were treated consecutively by steam-vapor extraction, biodegradation, and acid washing. The strain was identified as Pseudomonas aeruginosa, and named as Pseudomonas aeruginosa TPH1. The optimal culture conditions of TPH1 were $20^{\circ}C$ and pH 7.0, 3% of diesel concentration. Biodegradation of diesel was performed using the separated strain in liquid medium, and 63% of diesel was degraded in 72 hours. And 52% of diesel was removed in the tested soils. In the treatment of contaminated soils with diesel and Zn or As, 29% ~ 44% of diesel was reduced by steamvapor extraction, 60% ~ 71% of diesel was removed after biodegradation. 47% of Zn and 96% of As were removed after acid(mixture of sulfuric and oxalic acids) washing. It is recommended that consecutive treatment method of steam-vapor extraction, biodegradation and acid washing is effective for remediation of complex contaminated soils with metals and petroleum.

• Journal of Pharmaceutical Investigation
• /
• v.21 no.3
• /
• pp.171-177
• /
• 1991

A reverse-phase, ion-pair high performance liquid chromatographic (HPLC) method for the simultaneous quantative determination of pyridostigmine and its hydrolytic product, 3-hydroxy-N-methylpyridinium (HMP), is descrihed, The assay of pyridostigmine and HMP was linear in the range of amount from 24 to 60 mg/tablet and from 2.4 to 12.0 mg/tablet, respectively, with coefficient of variation (C.V.) of 0.05-0.12% (n=7) and 0.25-0.52% (n=5), respectively, and applicable conveniently even in the case of the mixture of pyridostigmine and HMP. Meanwhile, the conventional UV method gave inaccurate results for the aged pyridostigmine tablets. In the extraction of pyridostigmine from tablets prior to be assayed by HPLC, methanol was found to be more effective than ethanol or distilled water. Multiple extraction (four times) with methanol resulted in the full recovery of pyridostigmine, whereas ethanol gave 95% recovery even after four times extraction. Based on these results. the present method would be very useful for the accurate determination of pyridostigmine in the aged pyridostigmine tablets.

• Journal of Korean Society for Atmospheric Environment
• /
• v.24 no.3
• /
• pp.357-366
• /
• 2008

In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.