• Korean Journal of Medicinal Crop Science
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• v.22 no.2
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• pp.147-153
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• 2014

The Ponciri fructus immaturus (Poncirus trifoliata Rafinesque) has been used in oriental medicine for uterine contraction, stomachache, abdominal distension and cardiovascular diseases. Two main compounds, poncirin and naringin were successfully analyzed by high performance liquid chromatography (HPLC) and carried out method validation according to ICH guideline. A successful resolution and retention times were obtained with a $C_{18}$ reversed phase column, at an $1m{\ell}min^{-1}$ flow rate, with a gradient elution of a mixture of methanol, water and acetonitrile. Poncirin and naringin showed good linearity ($R^2$ > 0.999) in relatively wide concentration ranged. The recovery of each compound was 95.81 ~ 101.48% with R.S.D. values less than 1.0%. The application of ultrasound-assisted extraction was shown to be more efficient in extracting poncirin and naringin from Ponciri fructus immaturus. The predicted optimal poncirin and naringin yield were poncirin 2.15%, naringin 1.65% under an extraction temperature of $40^{\circ}C$, an extraction time of 10 min in a solvent of 70% methanol.

• Analytical Science and Technology
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• v.28 no.1
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• pp.1-7
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• 2015

4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), a tobacco specific nitrosamine found only in tobacco products. The ability to monitor biomarker concentrations is very important in understanding environmental tobacco smoke (ETS). In this study, an efficient and sensitive method for the analysis of NNK in dust was developed and validated using liquid chromatography tandem mass spectrometry. Dust was collected with filter paper soaked in methanol. The standard solution and dust sample were diluted with 100 mM ammonium acetate and extracted using dichloromethane. Our calibration curves ranged from 25 to $10^4pg/mL$. Excellent linearity was obtained with correlation coefficient values between 0.9996 and 1.0000. The limit of detection (LOD) was 5 pg/mL ($S/N{\geq}3$) and the retention time was 10 min. The limit of quantification (LOQ) was 25 pg/mL, and the acceptance criteria was the rate of 98-103% (80-120% at levels up to $3{\times}LOQ$). The coefficient of variations (CV) was 2.8%. Accuracies determined from dust samples spiked with four different levels of NNK racurves ranged that from 25 to 104 pg/mL. Excellent linearity was obtained between 92.1% and 114%. The precision of the method was acceptable (5% of CV). The recovery rates of the whole analytical procedure at low, medium, and high levels were 105.7-116.5% for NNK. The carry-over effects during LC-MS/MS analysis were not observed for NNK. This manuscript summarizes the scientific evidence on the use of markers to measure ETS.

• Analytical Science and Technology
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• v.30 no.1
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• pp.32-38
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• 2017

In attempt to contribute in official monographs of Korean Pharmacopoeia, an HPLC method was developed and fully validated for the determination of tolperisone hydrochloride in tablets which have never been published in other forgein Pharmacopoeia. Analysis was carried out in an ODS column ($250{\times}4.6mm$ I.D., $5{\mu}m$) with common solvents include acetonitrile and ammonium hydrophosphate buffer as mobile phase. The assay was validated according to International Conference on Harmonization (ICH) guidelines. The method has good linearity in the range of $5-200{\mu}g/mL$ tolperisone. Intra-day precision varied between 0.04 and 0.10 %. Relative standard deviations of inter-day precision ranged between 0.43 and 1.24 % for peak area. The percentage recovery of the tolperisone ranged between 99.8 and 101.2 % in material. Recoveries in tablets were ranged between 98.7 and 100.8 %, thus confirmed the suitability of method for estimation of tolperisone hydrochloride in tablet dosage form.

• Korean Journal of Food Science and Technology
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• v.42 no.5
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• pp.521-526
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• 2010

A high-performance liquid chromatography (HPLC) method was established for the determination of fluoroquinolones in milk. Protein was removed by using trichloroacetic acid in order to increase a mean recovery of milk. The extracts were using $Strata^{TM}$-X solid-phase extraction cartridge. The analytes were detected by HPLC on a $C_{18}$ column. HPLC method with fluorescence detection system (Ex: 278 nm, Em: 456 nm) provided a high degree of sensitivity in detecting fluoroquinolones. The limits of quantitation (LOQ) and mean recoveries of fluoroquinolones were 40 ${\mu}g$/kg and 73.6-95.2% (ofloxacin), 10 ${\mu}g$/kg and 77.3-91.9% (norfloxacin), 20 ${\mu}g$/kg and 91.6-94.3% (ciprofloxacin), 10 ${\mu}g$/kg and 81.0-87.8% (enrofloxacin), 10 ${\mu}g$/kg and 71.3-81.0% (sarafloxacin), 10 ${\mu}g$/kg and 89.4-90.8% (orbifloxacin), 2 ${\mu}g$/kg and 69.4-85.5% (danofloxacin).

• Korean Journal of Fisheries and Aquatic Sciences
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• v.38 no.6
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• pp.372-378
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• 2005

An analysis method of tetracyclines far fish and shellfish products containing large amount of low molecular materials and pigments was established. The recovery of the established analysis method for four tetracycline samples was $72-100\%$ and higher than other methods reported. Especially, proposed sample treatment protocol was shown to be effective for the removal of low molecular materials and pigments that tend to interfere with accurate analysis. The detection limit of oxytetracycline (OTC) and tetracycline (TC) from the sample was 0.02 ppm, and the detection limit of chlortetracycline (CTC) and doxycycline (DC) from the sample was 0.1ppm, To examine the efficiency of the established method and identify tetracycline usage in fish farms, tetracycline group antibiotics in the flounder being cultured was monitored. The improved method can be used for fish and shellfish products effectively and all surveyed fish farms have used tetracycline all the year round. The proposed method was adopted as official method for fishery products by Korean Food and Drug Administration in 2003 and it is being used by regulatory authority as National Fishery Products Quality Inspection Service.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.38 no.6
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• pp.379-384
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• 2005

A high-performance liquid chromatography assay method for oxolinic acid in fish products was developed, evaluated and validated through the monitoring of oxolinic acid based on farming and distribution. The recovery rate of the developed method was $102.3-106.7\%$ as compared to conventional methods. The stock solution was stable for 3 weeks under refrigerated condition at $4^{\circ}C$ The performance limit was evaluated as 0.01ppm of oxolinic acid in fish muscle. 478 fish samples such as olive flounder, genuine porgy, common sea bass and black rock fish collected from fish farms in the coastal area from September 2001 to October 2004 were analyzed to evaluate overall efficiency of the modified method and to monitor the actual condition of oxolinic acid usage in fish farm. According to the monitoring results, the modified method was suitable for analysis of oxolinic acid in fish muscle and oxolinic acid might be used in a small portion of fish farms. The suggested analysis method of oxolinic acid was registered in the Korean Official Methods of Food Analysis and is being utilized for fishery products by the Korea Food and Drug Adminstration and the National Fisheries Products Quality Inspection Service.

• Nuclear Engineering and Technology
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• v.49 no.8
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• pp.1711-1716
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• 2017

Uranium tetrafluoride ($UF_4$) is the most used nuclear material for producing metallic uranium by reduction with Ca or Mg. Metallic uranium is a raw material for the manufacture of uranium silicide, $U_3Si_2$, which is the most suitable uranium compound for use as nuclear fuel for research reactors. By contrast, ammonium uranyl carbonate is a traditional uranium compound used for manufacturing uranium dioxide $UO_2$ fuel for nuclear power reactors or $U_3O_8-Al$ dispersion fuel for nuclear research reactors. This work describes a procedure for recovering uranium and ammonium fluoride ($NH_4F$) from a liquid residue generated during the production routine of ammonium uranyl carbonate, ending with $UF_4$ as a final product. The residue, consisting of a solution containing high concentrations of ammonium ($NH_4^+$), fluoride ($F^-$), and carbonate ($CO_3^{2-}$), has significant concentrations of uranium as $UO_2^{2+}$. From this residue, the proposed procedure consists of precipitating ammonium peroxide fluorouranate (APOFU) and $NH_4F$, while recovering the major part of uranium. Further, the remaining solution is concentrated by heating, and ammonium bifluoride ($NH_4HF_2$) is precipitated. As a final step, $NH_4HF_2$ is added to $UO_2$, inducing fluoridation and decomposition, resulting in $UF_4$ with adequate properties for metallic uranium manufacture.

• Bulletin of the Korean Chemical Society
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• v.34 no.4
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• pp.1131-1136
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• 2013

Parabens, the esters of p-hydroxybenzoic acid, have been widely used as antimicrobial preservatives in cosmetic products, drugs, and processed foods and beverages. However, some parabens have been shown to have weak estrogenic effects through in vivo and in vitro studies. Because such widespread use has raised concerns about the potential human health risks associated with exposure to parabens, we developed a simultaneous analytical method to quantify 4 parabens (methyl, ethyl, propyl, and butyl) in human urine, by using solid-phase extraction and high-performance liquid chromatography coupled with triple quadrupole mass spectrometry. This method showed good specificity, linearity ($R^2$ > 0.999), accuracy (92.2-112.4%), precision (0.9-9.6%, CV), and recovery (95.7-102.0%). The LOQs for the 4 parabens were 1.0, 0.5, 0.2, and 0.5 ng/mL, respectively. This method could be used for quick and accurate analysis of a large number of human samples in epidemiological studies to assess the prevalence of human exposure to parabens.

• Korean Journal of Food Science and Technology
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• v.26 no.5
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• pp.633-637
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• 1994

A bacterial strain KSM-35 producing maltotetraose forming amylase was isolated from compost and identified as Streptomyces based on its morphological, cultural, and physiological characteristics. The amylase from Streptomyces sp. KSM-35 culture filtrate was purified by ammonium sulfate precipitation, followed by the liquid chromatographic procedures using DEAE-Toyo pearl and sephadex G-100 with 27.1% activity recovery. The molecular weight of the enzyme was estimated to be 50,000 and the isoelectric point 4.3. The main product by the amylase from soluble starch was maltotetraose which accounted for 56% of all the oligosaccharides detected after 26 hrs of reaction. Maltose (20%o) and maltotriose (16%) were the next important byproducts while glucose and maltopentaose were detected as traces.

• Journal of the Korean Applied Science and Technology
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• v.28 no.2
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• pp.135-139
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• 2011

In order to make high-purity ferro-manganese from $Mn_3O_4$ waste dust, the application of aluminothermite process to the reduction of the waste dust was investigated. The mixture from $Mn_3O_4$ dust as metallic source and Al metal powder as the reductant ignited, and reduced with an extremely intense exothermic reaction. The rapid propagation of the aluminothermite reaction occurred spontaneously and stably by ignition of the mixture. The Manganese having some alloy elements emerged as liquids due to the high temperatures reached up to about $2,500^{\circ}C$ and separated from the liquid by their differences of specific gravity. The result of thermite reaction showed the fact that can be obtained high purity ferro-manganese which have over about 90% of manganese content and lower impurities such as C, P, S than those of KS D3712 specification. The recovery of manganese from $Mn_3O_4$ dust was lower level of about 65% than about 75% from manganese ore by electric furnace process, that is due to spatter loss because of its extremely intense thermite reaction. But it will be improved by the process designed to provide CaO as the cooler or to use the Al metal powder having larger particle size distribution.