• Title/Summary/Keyword: Ion chromatography system

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Simultaneous Identification/Determination System for Sildenafil, Homosildenafil, Vardenafil and Tadalafil as Adulterants in Foods (식품중 불법함유된 발기부전치료제 성분 검출을 위한 동시분석법 연구)

  • Jang, Jae-Hee;Park, Kun-Sang;Park, Hye-Kyung;Koo, Yong-Eui;Choi, Youn-Ju;Hwang, In-Kyung;Kim, Dai-Byung
    • Journal of Food Hygiene and Safety
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    • v.18 no.4
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    • pp.195-201
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    • 2003
  • An easily available, simultaneous identification/determination procedure for sildenafil, homosildenafil, tadalafil, vardenafil in adulterated health related foods was established by using a combination of three different analytical methods; thin layer chromatography(TLC), liquied chromatography-mass spectrometry (LC/MS) and high-performance liquied chromatography (HPLC)/photo-diode-array detector. The sample solution for TLC was applied to silica gel 60 $F_{254}$ plates with ethylacetate/acetonitrile/25%ammonia (90:10:5) as a developing solvent. Spots were located under UV radiation at 254 nm and dragendolfs reagent. Mass spectra of the compounds by LC/MS were investigated with electrospray ionization (ESI) interface, under positive ion mode. The HPLC analysis was performed on a column of capcell pack $C_{18}$ (UG120, 4.6${\times}$250mm I.D. 5 ${\mu}$m)with 0.1% sodium 1-hexansulfonate (in 0.1% phosphoric acid)/acetnitrile (73:27) as a mobile phase, and effluent was minitored with a photo-diode-applied to commercial foods, Sildenafil content was inthe range of 0.4mg/g~360.9 mg/g from 7 out of 35 samples. Homosildenafil content was in the range of 2.2 mg/g~336.0 mg/g from 7 out of 35 samples. Tadalafil content was 429.3 mg/g, 9.6 mg/500 mg from 2 out of 35 samples. The procedure described here is available for the screening of sildenafil, homosildenafil, tadalafil, vardenafil.

Corrosion Failure Analysis of Air Vents Installed at Heat Transport Pipe in District Heating System (지역난방수 공급관 에어벤트 부식 파손 분석)

  • Lee, Hyongjoon;Chae, Hobyung;Cho, Jeongmin;Kim, Woo Cheol;Jeong, Joon Cheol;Kim, Heesan;Kim, Jung-Gu;Lee, Soo Yeol
    • Corrosion Science and Technology
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    • v.19 no.4
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    • pp.189-195
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    • 2020
  • Two air vents situated on a heat transport pipe in district heating system were exposed to the same environment for 10 years. However, one air vent was more corroded than the other. It also had a hole on the top of the front-end pipe. Comparative analysis was performed for these air vents to identify the cause of corrosion and establish countermeasures. Through experimental observation of the damaged part and analyses of powders sampled from air vents, it was found that corrosion was initiated at the top of the front-end pipe. It then spread to the bottom. Energy dispersive X-ray spectroscopy results showed that potassium and chlorine were measured from the corroded product in the damaged air vent derived from rainwater and insulation, respectively. The temperature of the damaged air vent was maintained at 75 ~ 120 ℃ by heating water. Rainwater-soaked insulation around the front-end pipe had been hydrolyzed. Therefore, the damaged air vent was exposed to an environment in which corrosion under insulation could be facilitated. In addition, ion chromatography and inductively coupled plasma measurements indicated that the matrix of the damaged front-end pipe contained a higher manganese content which might have promoted corrosion under insulation.

Study on Thermal Properties of CdS - Embedded Poly(2-Acetamidoacrylic acid) Hydrogel Composite (CdS 나노입자틀 삽입한 Poly(2-Acetamidoacrylic acid) 수화젤 복합체의 열적 특성에 관한 연구)

  • Park, Chun-Ho;Ha, Eun-Ju;Jung, Jong-Mo;Lee, Jang-Oo;Paik, Hyun-Jong
    • Polymer(Korea)
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    • v.33 no.1
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    • pp.1-6
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    • 2009
  • We report the template-based synthesis of well-dispersed CdS nanoparticles (NPs) in the interior of poly (2-acetamidoacrylic acid) (PAAA) hydrogel as a novel type of nanocomposite without particle aggregation via ion exchange in a aqueous system. As revealed by the TEM image analysis, the mean crystallite diameter of CdS NPs embedded in hydrogel composite was 4.5 nm, and the composite did not suffer any observable change after 6 months. Desorption/decomposition of CdS/PAAA hydrogel composite was studied by evolved gas analysis-gas chromatography-mass spectrometry (EGA-GC-MS), and thermogravimetric analysis (TGA) methods. From the TGA data, the thermal stability of the composite system increased by ca. 100 $^\circ$C and the content of CdS NPs in a dry composite gel was over 70 wt%. In addition, the chemical pathway was proposed for the entire decomposition process.

Insect Resistance of Tobacco Plant Expressing CpBV-ELP1 Derived from a Polydnavirus (폴리드나바이러스 유래 CpBV-ELP1 발현 담배의 내충성)

  • Kim, Eunseong;Kim, Yonggyun
    • Korean journal of applied entomology
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    • v.56 no.1
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    • pp.19-28
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    • 2017
  • Polydnaviruses (PDVs) are a group of double-stranded DNA viruses symbiotic to some endoparasitoid wasps. Cotesia plutellae bracovirus (CpBV) is a PDV symbiotic to an endoparasitoid wasp, C. plutellae, parasitizing young larvae of Plutella xylostella. An early expressed gene, CpBV-ELP1, plays an important role in the parasitism by suppressing host cellular immunity by its cytotoxic activity against hemocytes. This study aimed to test its oral toxicity against insect pest by expressing it in a recombinant tobacco plant. A recombinant CpBV-ELP1 protein was produced using a baculovirus expression system and secreted to cell culture medium. The cell cultured media were used to purify CpBV-ELP1 by a sequential array of purification steps: ammonium sulfate fractionation, size exclusion chromatography, and ion exchange chromatography. Purified rCpBV-ELP1 exhibited a significant cytotoxicity against Spodoptera exigua hemocytes. CpBV-ELP1 was highly toxic to the fifth instar larvae of S. exigua by injection to hemocoel. It also showed a significant oral toxicity to fifth instar larvae of S. exigua by a leaf-dipping assay. CpBV-ELP1 was cloned into pBI121 vector under CaMV 35S promoter with opaline synthase terminator. Resulting recombinant vector (pBI121-ELP1) was used to transform Agrobacterium tumefaciens LBA4404. The recombinant bacteria were then used to induce callus of a tobacco (Nicotiana tabacum Xanthi) leaves and subsequent generation (T1) plants were selected. T1 generation tobacco plants expressing CpBV-ELP1 gave significant insecticidal activities against S. exigua larvae. These results suggest that CpBV-ELP1 gene can be used to control insect pests by constructing transgenic crops.

Purified Polysaccharide Activating the Complement System from Leaves of Diospyos kaki L. (감잎(Diospyos kaki L.)으로부터 정제한 보체계 활성화 다당류)

  • Jung, Yung-Joo;Chun, Hyug;Kim, Kyung-Im;An, Jeung-Hee;Shin, Dong-Hoon;Hong, Bum-Shik;Cho, Hong-Yon;Yang, Han-Chul
    • Korean Journal of Food Science and Technology
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    • v.34 no.5
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    • pp.879-884
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    • 2002
  • Cold and hot water fractions of Diospyros kaki were screened to determine its anti-complementary activity. Flour of Diospyros kaki leaf (250 g) was boiled at $100^{\circ}C$ for 3 h and passed through a membrane of 10 kDa molecular weight (DK-0). DK-0 was precipitated with ethanol and refluxed with methanol to obtain the crude polysaccharide (DKC). DKC-1 was isolated by ion exchange chromatography on DEAE-Toyopearl 650C, and DKC-1c was purified from DKC-1 by size exclusion chromatography on Bio gel P-60. The anti-complementary activities of DKC-1c at $1000\;{\mu}g/mL$ were 85.4 and 61.1% via whole and alternative pathways, respectively. DKC-1c was determined as a neutral polysaccharide composed of glucose (29.0 mol.%), arabinose (24.3 mol.%), and galactose (16.2 mol.%) with the molecular weight of 66.6 kDa. Results of agarose gel immunoelectrophoresis revealed DKC-1c, as a complement activator, cleaved C3 into C3a and C3b via both pathways.

A Study on Interferences of Monochloramine in the Measurement of Ammonia by Phenate Method (Phenate 법으로 암모니아 분석시 염화아민의 방해 작용에 관한 연구)

  • Yoon, Je-Yong;Lee, Sang-Duck
    • Journal of Korean Society of Water and Wastewater
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    • v.12 no.1
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    • pp.45-51
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    • 1998
  • The determinations of ammonia in water for drinking purpose served as one basis of judging the sanitary quality of water for a great many years. However, presently ammonia regulation varies depending on countries. In USA and Canada, ammonia is added to water for chloramination process. However, for korea, there is ammonia regulation of treated water in Korea which should not exceed 0.5mg/l as $NH_3-N$. There was a report exceeding 0.5mg/l of ammonia in chlorinated water when the famous drinking water contamination episode happened in the downstream of Nadong River, 1994. With lack of sewer distribution system and treatment plants of domestic wastes, many water treatment plants have a difficulty of complying with ammonia regulation in treated water. Breakpoint chlorination is usually performed to get rid of ammonia. The method which is allowed to measure ammonia in Korea is Phenate method. However, it would be undesirable to use Phenate method for measuring ammonia in chlorinated water if Phenate method would not differentiate ammonia from chloramine. A good possibility of interferences in measurement of ammonia exists because Phenate method include the step of the formation of chlorine and would not differentiate chloramine which is formed as a result of reaction between chlorine and ammonia. This study was on inaccuracy of Phenate method for measuring ammonia of chlorinated water when chloramine and ammonia coexist. This study found that Phenate method measured all chlormaine as ammonia. Ammonia measurement by ion chromatography confirmed this results. Finally, the result from this study suggests that ammonia measurement by Phenate method in chlorinated water should be revised accordingly.

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Toxicokinetics of 4-tert-octylphenol in rats (Rat에서의 Octylphenol의 독성동태 연구)

  • 손수정;강현구;이선우;서수경;박인숙;안미령;최홍석;조재민;손동환
    • Environmental Mutagens and Carcinogens
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    • v.21 no.2
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    • pp.122-127
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    • 2001
  • 4-tert-octylphenol (OP) is a surfactant additive widely used in the manufacture of a variety of detergents and plastic products. Also, OP is known to have estrogenic activity by interacting with development and functions of endocrine system. This study was carried out to obtain toxicokinetic parameters of OP in male Sprague-Dawley rats. Male rats were administered OP, by either single oral (gavage) applications of 50, 100 or 200 mg/kg body weight. or a single intravenous injections of 1, 5 or 10 mg/kg body weight. Blood samples taken at several time intervals after administration were obtained from the femoral artery. Analysis of blood samples for OP was performed by gas chromatography mass spectrometry (GC/MS). The detection limit of OP was 1.9 ng/$m\ell$ at SIM (selected ion monitoring) mode of GC/MS. Calibration curve for analysis of the concentrations of OP in plasma was (OP/butylphenol peak area ratio) = 0.0294 $\times$ (plasma cone.) + 0.028 ($r^2$= 0.9991). The OP plasma concentration was 3921 ng/$m\ell$ immediately after single intravenous application, decreased rapidly within 45 min, and was detectable at low concentration up to 6 hr after application. When administered orally in rats (50, 100 and 200 mg/kg), OP was detected in the blood early after gavage administration, indicating the rapid initial uptake from gastrointestinal tract, with Tmax obtained from 0.67~0.83 hr. Using the AUC (area under the curve) of plasma concentration vs. time, low oral bioavailabilities of 1.2, 5.0 and 5.3% were calculated for the 50, 100 and 200 mg/kg groups, respectively.

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Isolation and Characterization of Biopolymers Extracted from the Bark of Acanthopanax sessiliflorus and Their Anticomplement Activity

  • Jeong Sang-Chul;Yang Byung-Keun;Jeong Yong-Tae;Rao Koyyalamudi Sundar;Song Chi-Hyun
    • Journal of Microbiology and Biotechnology
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    • v.17 no.1
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    • pp.21-28
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    • 2007
  • The crude biopolymer (AS-S1) and endobiopolymer (AS-S2) were isolated from the dry stem bark of Acanthopanax sessiliflorus and tested for anti complement activity. The two potent anticomplement biopolymers, AS-1 and AS-2-Fr.I, were isolated by the combination of ion-exchange chromatography and gel filtration methods from the endo-biopolymers (AS-S2). The anticomplement activity of AS-1 (MW 12 kDa) and AS-2-Fr.I (MW 180 kDa) were found to be 84.4% and 100.0%, respectively, at the concentration of $25{\mu}g/ml$. Activated pathway of the complement system occurred in both classical and alternative pathways, as evidenced by crossed immunoelectrophoresis(CIEP), where a major pathway was detected to be the classical one. It was found that the anticomplement activities of the periodate oxidized were decreased significantly, but those of pronase digested biopolymers of AS-1 and AS-2-Fr.I were decreased very little. The AS-1 contained 2,4,6-tri-O-methyl-D-glucitol, 2,3,6-tri-O-methyl-D-galacitol, and 2,3,6-tri-O-methyl-D-galacitol, which indicated that AS-1 contained a $(1{\rightarrow}3),\;(1{\rightarrow}4)-linked$ glucopyranosyl residue and a $(1{\rightarrow}4)-linked$ galactosyl residue. AS-2-Fr.I contained mainly 2,4-di-O-methyl-D-mannitol and 2,3,4-tri-O-methyl-D-galacitol, which contained $(1{\rightarrow}3),\;(1{\rightarrow}6)$ linked mannosyl and $(1{\rightarrow}6)$ linked galactosyl residues.

Purification of Oxytocin-related Peptide, Isotocin from the Brain of Conger Eel Conger myriaster (붕장어(Conger myriaster)의 뇌로부터 Oxytocin-related Peptide, Isotocin의 정제)

  • GO Hye-Jin;KIM Chan-Hee;KIM Eun Jung;KIM In Hae;AN Sang Hyun;SOHN Hee-Young;PARK Jin-IL;PARK HEE Yun;YOON Ho Dong;PARK Nam Gyu
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.38 no.5
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    • pp.286-290
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    • 2005
  • Oxytocin (OT)-related peptide, isotocin was purified from the brain extract of conger eel (Conger myriaster) using reverse-phase, ion-exchange and size exclusion high performance liquid chromatography (HPLC). The sequence of the peptide, with a molecular weight of 967.30 Da, was determined as Cys-Tyr-Ile-Ser-Asn­Cys-Pro-Ile-Gly-$NH_2$, where the Cys between 1st and 6th residues made an intramolecular disulfide bridge by the automated amino acid sequence analysis and MALDI-TOF mass spectrometry. The sequence was confirmed by identical elution with the purified and synthetic peptide using the HPLC system. As a result of homology investigation, the primary structure of this peptide was the same as that of OT -superfamily member, isotocin. The synthetic peptide showed a contractile activity at a minimal effective concentration of $10^{-7}M$ on the intestinal smooth muscle of goldfish (Carassius auratus).

Preparation and Analysis of Yeast Cell Wall Mannoproteins, Immune Enhancing Materials, from Cell Wall Mutant Saccharomyces cerevisiae

  • Ha Chang-Hoon;Yun Cheol-Won;Paik Hyun-Dong;Kim Seung-Wook;Kang Chang-Won;Hwang Han-Joon;Chang Hyo-Ihl
    • Journal of Microbiology and Biotechnology
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    • v.16 no.2
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    • pp.247-255
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    • 2006
  • Yeast cell wall matrix particles are composed entirely of mannoprotein and ${\beta}-glucan$. The mannoproteins of yeast cell wall can systemically enhance the immune system. We previously purified and analyzed alkali-soluble ${\beta}-glucans$ [${\beta}$-(1,3)- and ${\beta}$-(1,6)-glucans] [10]. In the present study, a wild-type strain was first mutagenized with ultraviolet light, and the cell wall mutants were then selected by treatment with 1.0 mg/ml laminarinase (endo-${\beta}$-(1,3)-D-glucanase). Mannoproteins of Saccharomyces cerevisiae were released by laminarinase, purified by concanavalin-A affinity and ion-exchange chromatography. The results indicated that the mutants yielded 3-fold more mannoprotein than the wild-type. The mannoprotein mass of mutant K48L3 was 2.25 mg/100 mg of yeast cell dry mass. Carbohydrate analysis revealed that they contained mannose, glucose, and N-acetylglucosamine. Saccharomyces cerevisiae cell wall components, mannoproteins, are known to interact with macrophages through receptors, thereby inducing release of tumor necrosis factor alpha ($TNF-{\alpha}$) and nitric oxide. Mannoprotein tractions in the present study had a higher macrophage activity of secretion of $TNF-{\alpha}$ and nitric oxide and direct phagocytosis than positive control ($1{\mu}g$ of lipopolysaccharide). In particular, F1 and F3 fractions in mannoproteins of K48L3 enhanced and upregulated the activity of nitric oxide secretion and macrophage phagocytosis by approximately two- and four-fold, respectively.