• Title/Summary/Keyword: A new reagent

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Determination of Protoberberine Alkaloids in Phellodendri Cortex and Preparation by Spectrophotometric Method (흡광도측정법에 의한 황백과 제제 중 프로토베르베린 알칼로이드의 정량)

  • 엄동옥;정윤철
    • YAKHAK HOEJI
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    • v.45 no.1
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    • pp.34-38
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    • 2001
  • The Phellodendri Cortex of Phellodendron amurense (Rutaceae) is known to contain a number of isoquinoline alkaloid, and berberine, palmatine, jateorrhizine, phellodendrine and magnoflorine are the major constituents of protoberberine alkaloids. For the determination of protoberberine alkaloids from Phellodendri Cortex and berberine chloride from the preparation, the new spectrophotometric method was developed with a simple and selective sample clean-up using thiocyanatocobaltate[II] complex ion. Samples were extracted with 0.1 mM hydrochloric acid, potassium biphthalate reagent, thiocyanatocobaltate reagent and 1.2-dichloroethane for 60 min. The absorbance of protoberberine alkaloid complexes in 1.2-dichloroethane solution was measured at 625 nm. Calibration curve for berberine was linear over the concentration range of 0.05~0.30 mg/ml 1.2-dichloroethane. The method proved to be rapid, simple and reliable for the determination of protoberberine alkaloids from Phellodendri Cortex and berberine chloride from the preparation.

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Synthesis of Acyclic Nucleosides of 2-Thio-Pyrimidines and -Purines Using a New Coupling Agent of Lithium Bromide

  • Kim, Joong-Young;Kim, Yong-Hae
    • Bulletin of the Korean Chemical Society
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    • v.9 no.5
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    • pp.295-298
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    • 1988
  • Acyclic nucleosides, 1-[[1,3-bis(benzyloxy)-2-propoxy]methyl]-2-thiopyrimidine, 9-[[1,3-bis(benzyloxy)-2-propoxy]methyl]-6-amino -2-thiopurine, 1-(2-acetoxyethoxymethyl)-2-thiopyrimidine, and 9-[[1,3-bis(benzyloxy)-2-propoxy]methyl]-6-amino -2-thiopurine have been synthesized by coupling pyrimidine and purine bases with acyclic acetates using a new coupling reagent of lithium bromide in the presence of trifluoro acetic acid in acetonitrile.

STUDY ON GY NEW MINERAL PROCESSING TECHNOLOGY FOR SHIZHUYUAN POLYMETALLIC ORE

  • Zhang, Zhonghan;Li, Xiaodong;Ye, Zhiping;Guo, Jianguan
    • Proceedings of the IEEK Conference
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    • 2001.10a
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    • pp.325-330
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    • 2001
  • Shizhuyuan W-Mo-Bi-Ca $F_2$polymetallic ore is classified to the refractory one due to its complex property, fine dissemination and close association of minerals. Through several years of researches, in line with GY new mineral processing technology developed by Guangzhou Research Institute of Nonferrous Metals, in sulfide flotation circuit, an iso-flotability flowsheet is used to replace original overall bulk flotation flowsheet, and in tungsten flotation circuit, a new chelating type-GY reagent and a special pulp-conditioning system and a new technology of wolframite slime flotation are used to replace the traditional "Caustic Soda Method"$_{[1]}$, the metallurgical performance is greatly improved. Besides, GY New Method has created a favorable condition for comprehensive recovery of fluoride from tungsten flotation tailings. Notable economic benefit has been achieved.d.

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Indirect Determination of Nitrite by Flame Atomic Absorption Spectrometry Using a Lead(IV) Dioxide Oxidant Microcolumn

  • Noroozifar, Meissam;Khorasani Motlagh, Mozhgan;Taheri, Aboozar;Homayoonfard, Marjan
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.875-880
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    • 2006
  • A new, simple and fast flow injection analysis (FIA) method has been developed for the indirect determination of nitrite. The proposed indirect automatic method is based on the oxidation of nitrite to nitrate using a lead(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the $PbO_2$ solid phase reagent to Pb(II), which is measured by flame atomic absorption spectrometry. The absorbance of Pb(II) are proportional to the concentration of nitrite in the samples. The calibration curve was linear up to 30 mg $L ^{-1}$, with a detection limit of 0.11 mg $L ^{-1}$ for a 400 mL injected sample volume and a sampling rate of about 80 $h ^{-1}$. The results exhibit no interference from the presence of large amounts of ions. The developed procedure was found to be suitable for the determination of nitrite in foodstuffs and wastewaters. A relative standard deviation better than 0.9% was obtained in a repeatability study. The reliability of the method was established by parallel determination against the standard method.

An Expeditious Oxidative Aromatization of Hantzsch 1,4-Dihydropyridines to Pyridines Using Cetyltrimethylammonium Peroxodisulfate: A Phase Transferring Oxidant

  • Kumar, Parvin;Kumar, Ashwani
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2299-2303
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    • 2010
  • A new approach to the use of potassium peroxodisulphate as an oxidizing reagent is proposed and applied to the case of oxidative aromatization of 1, 4-dihydropyridines with cetyltrimethylammonium peroxodisulfate, a phase transfer oxidant. We demonstrate how it is possible to increase the reactivity of potassium peroxodisulphate in the presence of phase transfer catalyst. Dealkylation in case of 4-n-alkyl/n-alkenyl was not obtained.

Beckmann Rearrangement of Ring A Steroidal Oxime Using the Carbon tetrachloride-triphenylphosphine (사염화탄소와 트리페닐포스핀을 사용한 스테로이드 링 A 옥심의 벡크만 자리옮김반응)

  • Kim Jack C.;Choi Soon-Kyu;Park Won-Woo;Lee Yong-Tae
    • Journal of the Korean Chemical Society
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    • v.23 no.1
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    • pp.42-45
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    • 1979
  • The experimental procedures of Beckmann rearrangement mostly involve the use of vigorous conditions such as strongly acidic reagents (conc. HCl, $H_2SO_4$, $PCl_5$, etc.) or elevated temperatures, which frequently cause isomerization of ketooximes prior to rearrangement.We have effected the Beckmann rearrangement on $5{\alpha}$-cholestan-3-one oxime using the carbon tetrachloride-triphenylphosphine reagent under mild, neutral conditions to give 3-aza-A-homo-$5{\alpha}$-cholestan-4-one. This new, mild, facile and rapid general method of Beckmann rearrangement is presented, and compared with the classical (more conventional) Beckmann reagent of polyphosphoric acid.

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Radioimmunoassay Reagent Survey and Evaluation (검사별 radioimmunoassay시약 조사 및 비교실험)

  • Kim, Ji-Na;An, Jae-seok;Jeon, Young-woo;Yoon, Sang-hyuk;Kim, Yoon-cheol
    • The Korean Journal of Nuclear Medicine Technology
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    • v.25 no.1
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    • pp.34-40
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    • 2021
  • Purpose If a new test is introduced or reagents are changed in the laboratory of a medical institution, the characteristics of the test should be analyzed according to the procedure and the assessment of reagents should be made. However, several necessary conditions must be met to perform all required comparative evaluations, first enough samples should be prepared for each test, and secondly, various reagents applicable to the comparative evaluations must be supplied. Even if enough comparative evaluations have been done, there is a limit to the fact that the data variation for the new reagent represents the overall patient data variation, The fact puts a burden on the laboratory to the change the reagent. Due to these various difficulties, reagent changes in the laboratory are limited. In order to introduce a competitive bid, the institute conducted a full investigation of Radioimmunoassay(RIA) reagents for each test and established the range of reagents available in the laboratory through comparative evaluations. We wanted to share this process. Materials and Methods There are 20 items of tests conducted in our laboratory except for consignment tests. For each test, RIA reagents that can be used were fully investigated with the reference to external quality control report. and the manuals for each reagent were obtained. Each reagent was checked for the manual to check the test method, Incubation time, sample volume needed for the test. After that, the primary selection was made according to whether it was available in this laboratory. The primary selected reagents were supplied with 2kits based on 100tests, and the data correlation test, sensitivity measurement, recovery rate measurement, and dilution test were conducted. The secondary selection was performed according to the results of the comparative evaluation. The reagents that passed the primary and secondary selections were submitted to the competitive bidding list. In the case of reagent is designated as a singular, we submitted a explanatory statement with the data obtained during the primary and secondary selection processes. Results Excluded from the primary selection was the case where TAT was expected to be delayed at the moment, and it was impossible to apply to our equipment due to the large volume of reagents used during the test. In the primary selection, there were five items which only one reagent was available.(squamous cell carcinoma Ag(SCC Ag), β-human chorionic gonadotropin(β-HCG), vitamin B12, folate, free testosterone), two reagents were available(CA19-9, CA125, CA72-4, ferritin, thyroglobulin antibody(TG Ab), microsomal antibody(Mic Ab), thyroid stimulating hormone-receptor-antibody(TSH-R-Ab), calcitonin), three reagents were available (triiodothyronine(T3), Tree T3, Free T4, TSH, intact parathyroid hormone(intact PTH)) and four reagents were available are carcinoembryonic antigen(CEA), TG. In the secondary selection, there were eight items which only one reagent was available.(ferritin, TG, CA19-9, SCC, β-HCG, vitaminB12, folate, free testosterone), two reagents were available(TG Ab, Mic Ab, TSH-R-Ab, CA125, CA72-4, intact PTH, calcitonin), three reagents were available(T3, Tree T3, Free T4, TSH, CEA). Reasons excluded from the secondary selection were the lack of reagent supply for comparative evaluations, the problems with data reproducibility, and the inability to accept data variations. The most problematic part of comparative evaluations was sample collection. It didn't matter if the number of samples requested was large and the capacity needed for the test was small. It was difficult to collect various concentration samples in the case of a small number of tests(100 cases per month or less), and it was difficult to conduct a recovery rate test in the case of a relatively large volume of samples required for a single test(more than 100 uL). In addition, the lack of dilution solution or standard zero material for sensitivity measurement or dilution tests was one of the problems. Conclusion Comparative evaluation for changing test reagents require appropriate preparation time to collect diverse and sufficient samples. In addition, setting the total sample volume and reagent volume range required for comparative evaluations, depending on the sample volume and reagent volume required for one test, will reduce the burden of sample collection and planning for each comparative evaluation.

Studies on the Fluorophotometric Determination of Gentamicin Sulfate and its Preparations (Gentamicin Sulfate의 형광분석법에 관한 연구)

  • 백우현;김정우;허명권;박근창
    • YAKHAK HOEJI
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    • v.22 no.1
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    • pp.15-21
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    • 1978
  • Gentamicin sulfate reacted with pyridoxal and zinc (II) ion in pyridine-methanol solution to yield highly fluorescent zinc(II) chelates of N-pyridoxylidene derivatives. This fluorescence reaction was sensitive and showed excitation maximum at 398nm, and emission maximum at 482nm. The effects of reagent concentration, reaction time and temperature, standing time and temperature were studied. And a new fluorophotometric method for the determination of gentamicin sulfate was developed. A good result was obtained and this method was applied to various preparations.

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1-Methylimidazolium Chlorochromate. A New Efficient Oxidizing Agent for Oxidation of Alcohols and Oxidative Cleavage of Oximes

  • Kim, Sung-Gak;Chang, Heung
    • Bulletin of the Korean Chemical Society
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    • v.8 no.3
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    • pp.183-185
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    • 1987
  • 1-Methylimidazolium chlorochromate was prepared by the addition of 1-methylimidazole into a solution of chromic trioxide in 6M hydrochloric acid and obtained in high yield as bright yellow crystalline solids. The reagent was found to be very effective for the oxidation of alcohols and the oxidative cleavage of oximes to the corresponding carbonyl compounds.