• Title/Summary/Keyword: Distillation extraction

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Study on Isolative Determination Methylephedrine Hydrochloride and Ephedrine Hydrochloride in the Mixed Preparation (혼합제제중 Methylephedrine Hydrochloride와 Ephedrine Hydrochloride의 분리정량에 관한 연구)

  • Ko, In-Suk
    • Korean Journal of Pharmacognosy
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    • v.1 no.3
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    • pp.93-99
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    • 1970
  • There have been reported by several workers for the isolation and determination of the amine derivatives as Metbylephedrine Hydrochloride and Ephedrine Hydrochloride adopting neutralization method, steam distillation method, non-aqous titration method, ion-exchange resin method, titration method after acetylation, colorimetric method, gravimetric method, iodine titration method and gas chromatography. Those methods mentioned in above, can be practically applied for the sample which is not mixed one mith the other amine compounds. Presently, it has not shown on the isolative determination of the mixed sample of amine derivatives. In this paper, it is discussed on the isolative determination of Methylephedrine Hydrochloride as the tertiary amine compound and Ephedrine Hydrochloride as the secondary amine compound. According to the results of the experiment, it could be summarized as follows: 1. There is no time-variation on the color reaction of Methylephedrine Hydrochloride and Ephedrine Hydrochloride with the color reagent, bromcresolgreen. And Methylephedrine Hydrochloride and Ephedrine Hydrochloride, respectively, can be determined spectrophotometrically by means oft his color reaction. 2. For the isolation of Methylephedrine Hydrochloride and Ephedrine Hydrochloride from the mixed sample, Methylephedrine Hydrochloride can be eluted by chloroform, while Ephedrine Hydrochloride by the mixed solvent of chloroform and ethylalcohol (2:1), from the celite column adsorbed at pH6.4 followed by extraction with ether undersodium hydroxide alkali re action. 3. When the sample is mixed with quinine hydrochloride, dihydrocodeine bitartate, and noscapine, these mixed compounds can be eliminated by means of stram distillation. 4. When the sample is mixed with chlorpheniramine maleate, dextromethorphan hydrobromide and diphenhydramine hydrochloride, the mixed compounds can be eliminated by means of steam distillation and celite adsorption column chromatography, In conclusion, the isolative determination method for Methylephedrine Hydrochloride and Ephedrine Hydrochloride studied in this paper, indicates with the excellent reproducibility and accuracy.

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Analysis of Soil Total Nitrogen and Inorganic Nitrogen Content for Evaluating Nitrogen Dynamics

  • Lee, Seul-Bi;Sung, Jwa-Kyung;Lee, Ye-Jin;Lim, Jung-Eun;Song, Yo-Sung;Lee, Deog-Bae;Hong, Suk-Young
    • Korean Journal of Soil Science and Fertilizer
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    • v.50 no.2
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    • pp.100-105
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    • 2017
  • Various methods for assessing soil total nitrogen (TN) and inorganic N content have been developed to manage nutrient and to understand N cycle in soil. This paper address the technical procedures in arable soil samples to conduct soil sampling, sample preparation, and measuring total N and inorganic N. Among various methods for measuring soil total nitrogen contents, Kjeldahl distillation and Indophenol blue method have widely used due to reliability and economic advances. Also, two methods can analyze more samples at the same time compared with other nitrogen measuring methods. For evaluating inorganic N content, mainly in forms of nitrate-N ($NO_3{^-}-N$) and ammonium-N ($NH_4{^+}-N$), extraction with a single reagent such as 2M KCl has been employed, followed by Kjeldahl distillation or indophenol blue methods.

A study for cyclic Process technique of mineral base engine used oil resource (Engine 폐유 자원순환 기술에 관한 연구)

  • 김주항
    • Journal of the Korean Professional Engineers Association
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    • v.18 no.2
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    • pp.6-15
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    • 1985
  • A new process disregraded the H$_2$SO$_4$ treatment process heretofore in use, was developed and substituted for mineral base engine used oil of homemade SAE-30 grade H.V.I., which was used covering 4,500km, as samples, and the following results in research, was obtained. (1) A good quality of rerefinded base oil was obtained through roughly a course of developed processes of vacuum distillation process, solvent extraction process, neutralization treatment process and clay treatment process. (2) Through vacuum distillation process, the size of fine grains of insoluble colloid carbon that is, colloid carbon which was produced by burning of internal combustion engine oil and fuel, could be brought up and precipitated (3) The insoluble matters and admixtures could be easily dispersed and dissolved by mixing and extracting solvent disregarded the H$_2$SO$_4$ treatment process heretofore in use (4) waste matter heretofore called acid sludge in consequence of the process, did not appear at all. accordingly, the environmental pollution could be removed. (5) The troubles of corrosion to copper strip which was faults of the usual used oil refined products and peculiar offensive odor of the rerefined oil, could be solved through the neutralization process. (6) The yield of rerefined oil obtained through a course of processes was over 86 percent, and it is of practical use, not to speak of commercial value.

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Qualitative, Quantitative Analysis and Chiral Characterization of the Essential Oils of Juniperus phoenicea L. and Juniperus oxycedrus L.

  • Dahmane, Dahmane;Dahmane, Fahima Abdellatif;Dob, Tahar;Chelghoum, Chaabane
    • Natural Product Sciences
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    • v.26 no.1
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    • pp.97-107
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    • 2020
  • Isolation of oils from leaves of Juniperus phoenicea and Juniperus oxycedrus was obtained by steam distillation extraction method. The compositions of essential oils (EOs) were studied by means of GC-MS and GC-FID, using the internal standard method and relative response factors. Around ninety eight compounds were determined in total, representing 98.25 g/100 g of EO of J. phoenicea and 98.48 g/100 g of EO of J. oxycedrus, respectively. The volatile leaf oils were dominated by the terpenic hydrocarbon fractions (79.87 g/100 g) and (61.27 g/100 g) characterized by high contents of α-pinene (64.6 g/100 g) and (54.0 g/100 g) in J. phoenicea and J. oxycedrus, respectively, as the main component. Also, the enantiomeric distribution of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, linalool, terpinen-4-ol, bornyl acetate, and borneol in both oils is presented for the first time.

Essential Oil Composition of Umbelliferous Herbs (미나리과 허브식물의 향기성분)

  • 홍철운;김명곤;김철생;김남균
    • The Korean Journal of Food And Nutrition
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    • v.14 no.1
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    • pp.10-14
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    • 2001
  • The volatile components of umbelliferous herbs having a characteristic spicy aroma were investigated. The essential oils of herbs were isolated by simultaneous steam distillation and extraction and the volatile components were identified by capillary GC and GC/MS. Forty-nine volatile compounds were identified from the herbs. The major compounds of chervil (Anthricus cerefolium) leaf oil were methyl chavicol, 1-allyl-2,4-dimethoxy benzene, and of coriander (Coriandrum sativum) leaf oil were ${\beta}$-sesquiphellan drene, germacrene B, nerolidol, selinene-4-ol, and of coriander seed oil were linalool, decanal, ${\gamma}$-terpinene, $\rho$-cymene.

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Studies on the Manufacturing of Carbonaceous Products (Ⅰ) Effects of the Binder by Cutting Condition of Coal Tar (炭素製品 製造에 關한 硏究 (第 1 報) Coal tar의 Cutting 條件에 依한 粘結劑로서의 檢討)

  • Won Dal Hyun;Ju Seong Lee;Hi Wook Kim
    • Journal of the Korean Chemical Society
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    • v.8 no.3
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    • pp.98-102
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    • 1964
  • As a practical method to produce the carbonaceous binder, the destructive distillation of coal tar has been studied. The optimum condition on binder in various temp. and cutting time were examined and the compositions of pitch were also examined in connection with ${\alpha},\;{\beta}\;and\;{\gamma}$ by solvent extraction. Coke powder was mixed with binder as treated pitch in the proportions of 77% of coke to 23% of pitch, to give a plastic mix which could then be pressed into molding. The properties of baked body after molding was tested. It was found that cutting of the coal tar at 350${\circ}C$, for 30 min., at 300${\circ}C$. for 1 hr., and at 250${\circ}C$. for 8 hrs. were good condition. Particularly, we found that the cutting of the coal tar obtained by destructive distillation at high temp. and in minimum period of time had shown the best condition for utilization of carbonaceous pitch as binder. The above mentioned cutting condition results in good quality of pitch which is available to be used as binder in carbon industry.

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GC/MS and HPLC/PDA characterization of essential oils and phenolic compounds from the aerial parts of common rue (Ruta graveolens)

  • Chang-Dae Lee;Hak-Dong Lee;Yunji Lee;Hwan Myung Lee;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.144-152
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    • 2023
  • Two different extraction methods were used to evaluate the medical value of common rue, Ruta graveolens L. (RGL). The results of our 2,2-diphenyl-1-picrylhydrazyl and 2,2'-azino-bis-3-ethylbenzothiazoline-6-sulphonic acid assays indicated that the antioxidant activity of RGL essential oil extract obtained through steam distillation was very low, whereas ethanol (EtOH) extracts of RGL showed higher antioxidant activity. RGL essential oil was extracted by steam distillation and characterized by GC/MS analysis. Furthermore, EtOH extracts of RGL were obtained under reflux and analyzed by HPLC/PDA. The GC/MS results indicated that the ketone compounds 2-undecanol acetate, nonyl cyclopropanecarboxylate, and 2-nonanone accounted for more than 70% of the composition of RGL essential oil. The HPLC/PDA analyses indicated that the RGL extracts were rich in phenolic compounds such as protocatechuic acid, rutin, psoralen, xanthotoxin, and bergapten, among which rutin was the most abundant. Collectively, our results demonstrated that RGL contains high levels of phenolic compounds and could thus be commercialized as a valuable plant-derived antioxidant.

Determination of Methylmercury in Biological Samples Using Dithizone Extraction Method Followed by Purge & Trap GC-MS

  • Lee, Jung-Sub;Ryu, Yoon-Jung;Park, Jae-Sung;Jeon, Sung-Hwan;Kim, Sam-Cwan;Kim, Young-Hee
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2293-2298
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    • 2007
  • In this study, a dithizone extraction technique involving purge & trap GC-MS was developed for the determination of methylmercury in biological samples, especially blood and fish. After alkaline digestion, methylmercury in biological samples was extracted into dithizone and back-extracted into aqueous sulfide solution. The extracted methylmercury was converted to the volatile ethyl derivative, purged and trapped onto a solid-phase collection medium, and then introduced into the GC-MS system. The determined MDLs of the established method were 0.9 ng·g?1 for biological samples and its accuracy and precision were found to be 93% and 3.8%, respectively. The method was validated by analysis of CRMs such as SRM 966, BCR 463 and IAEA 407 and all analytical results were within certified ranges with average RSDs of less than 6%. The analytical results of field-sampled fish also showed that the method can be successfully used as an alternative for commonly used distillation method followed by GC-CVAFS detection.

Analysis of Aroma Compounds of Cinnamon by Solid Phase Microextraction (Solid Phase Microextraction을 이용한 계피의 향기성분 분석)

  • 이창국;이재곤;장희진;곽재진
    • The Korean Journal of Food And Nutrition
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    • v.16 no.4
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    • pp.372-378
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    • 2003
  • The volatile components of cinnamon bark were extracted by using different isolation methods, simultaneous distillation extraction (SDE) and solid phase microextraction (SPME). Then the volatile components were analyzed by gas chromatography(GC) and mass selective detector(MSD). 30 compounds were identified in cinnamon bark. In SPME technique, several factors influencing the equilibrium of the aroma compounds between sample and SPME fiber was taken into account, including the kind of SPME fiber, extraction temperature and extraction time. Four different SPME fibers were tested, namely polydimethylsiloxane (PDMS), poly acrylate(PA), divinyl- benzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS) and carbowax/divinylbenzene(CW/DVB). Among these SPME fiber, PDMS coating fiber showed the best results. The profile of volatile compounds of cinnamon bark at different extraction temperature and extraction time were investigated by 100$\mu\textrm{m}$ PDMS fiber.

Optimization of d-limonene Extraction from Tangerine Peel in Various Solvents by Using Soxhlet Extractor (다양한 용매에서 Soxhlet 추출기를 이용한 감귤 껍질에서 d-limonene 추출의 최적조건 연구)

  • Park, Sang Min;Ko, Kwan Young;Kim, In Ho
    • Korean Chemical Engineering Research
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    • v.53 no.6
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    • pp.717-722
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    • 2015
  • D-limonene included in citrus fruits is obtainable to extract essential oil as well as separate the oil ingredient. Soxhlet extraction, a type of SDE (Simultaneous steam Distillation and solvent Extraction), was used to extract limonene from tangerine peel. HPLC analysis was performed to quantify extracted d-limonene by using reversed-phase HPLC column. Results of HPLC analysis showed that the optimal extraction time was 2 hours in any solvent, and the extracted amounts of d-limonene in tangerine peel (per g tangerine peel) were 7.77 mg, 0.49 mg, and 0.28 mg in ethyl alcohol, n-hexane, and ether. Because yield was the highest in using ethyl alcohol as a solvent, polarity is stronger factor to effect on yield of extraction than boiling point.