• Title/Summary/Keyword: 잔류 용매

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Removal of Residual Solvents in Paclitaxel by Supercritical Carbon Dioxide (초임계 이산화탄소를 이용한 Paclitaxel의 잔류용매 제거)

  • 김진현;박흥복;기은숙;강인선;최형균;홍승서
    • KSBB Journal
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    • v.16 no.3
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    • pp.233-236
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    • 2001
  • Because of casehardenign effect of amorphous paclitaxel, residual solvents, methylene chloride and emthanol could not be reduced to the maximum value allowed, 600 ppm and 3,000 ppm, in accord with the guidelines issued by the International Conference on Harmonization (ICH, 1997), using rotary evaporation and successive drying in a vacuum oven. However, methylene chloride and methanol were reduced to 486 ppm and 403 ppm, respectively using supercritical $CO_2$ on purified paclitaxel. The optimum pressure and operating time were 80 bar and 30 min at fixed operating temperature ($40^{circ}C$). This approach serves as a novel application of supercritical fluid extraction to remove residual solvents from active pharmaceutical ingredients.

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Ethanol-pretreated Drying of (+)-dihydromyricetin for Removal of Residual Solvents (잔류 용매 제거를 위한 (+)-dihydromyricetin의 에탄올 전처리 건조)

  • Lee, Hee-Gun;Kim, Jin-Hyun
    • Korean Chemical Engineering Research
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    • v.60 no.2
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    • pp.237-242
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    • 2022
  • In this study, a drying method that can effectively remove residual solvent from (+)-dihydromyricetin was developed. Residual acetone concentration was efficiently removed below ICH-specified value (5,000 ppm) by simple rotary evaporation with ethanol pretreatment. In addition, the residual ethanol met the ICH-specified value (5,000 ppm) by simple rotary evaporation through the addition of water, and the residual moisture also met the specified value (<4%) for active pharmaceutical ingredients. At all the drying temperature (35, 45, and 55 ℃), a large amount of the residual solvent was initially removed during the drying, and the drying efficiency increased when increasing the drying temperature. Removal of residual solvent by ethanol pretreatment was shown to be related to high vapor pressure of acetone-ethanol mixture and hydrogen bonding between acetone and ethanol.

A Study on Detection of Residual Solvent, Ethoxyquin and Color Stability in Oleoresin Paprika Extracts (파프리카 추출물의 색소안정성과 Ethoxyquin 및 잔류용매 검출)

  • Lee, Seon-Ok;Kyung, Suk-Hun;Park, Kil-Dong;Kang, Hee-Gon;Park, Joo-Sung;Lee, See-Kyung
    • Applied Biological Chemistry
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    • v.45 no.2
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    • pp.77-83
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    • 2002
  • Effects of ethoxyquin on the color stability of oleoresin paprika extracts and amount of residual ethoxyquin, a color stabilizer, in commercial extracts were determined. The oleoresin paprika extracts dissolved in ethanol gave the highest maximum photo-absorbency at 444-458 nm, with the color index of United States product 2-6 times higher than that produced in India. The residual solvents in oleoresin paprika extracts were mainly acetone and methanol, although some other extracts also contained small amounts of hexane. HPLC analysis was determined as a proper analytical method for residual ethoxyquin assay in the oleoresin paprika extracts, particularly when hexane was used as a solvent. The residual ethoxyquins were detected in the extracts produced in US and Spain which had relatively high color indices.

Analysis of Thermal Imidization Kinetics of 6FDA-BAPP Polyimide in Relation with Solvent Evaporation (6FDA-BAPP 폴리이미드 열축합 반응에서의 잔류용매에 따른 이미드화거동 연구)

  • Lee, Eun-Young;Hwang, Tae-Seon;Nam, Jae-Do
    • Polymer(Korea)
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    • v.36 no.4
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    • pp.448-454
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    • 2012
  • A poly(amic acid) (PAA) was prepared by reaction of 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluropropane (BAPP) in N,N-dimethylacetamide (DMAc). The cast films of the synthesized PAA were thermally treated at different temperatures to create polyimide (PI) films. The heat treatment temperature varied between 80 and $230^{\circ}C$ to investigate the imidization index in relation with the solvent evaporation rates. The progress of PAA imidization was examined using a thermogravimetric analyzer (TGA) and a Fourier transform infrared spectroscope (FTIR) at various time and temperature. The experimental results showed that the imidization index was fast at the initial stage in the presence of solvent, DMAc, reaching the final imidization. When the imidization temperature is high over $200^{\circ}C$, the imidization index decreased because the solvent was evaporated too fast.

Removal Efficiency of Pesticide Residues on Apples by Ultrasonic Cleaner (초음파 세척기를 이용한 사과의 잔류농약 제거 효과)

  • Yoon, Chae-Hyuk;Park, Woo-Churl;Kim, Jang-Eok;Kim, Chung-Hyo
    • Korean Journal of Environmental Agriculture
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    • v.16 no.3
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    • pp.255-258
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    • 1997
  • In order to determine the removal efficiency of pesticide residues on apples by ultrasonic cleaner, apples(Fuji var.) were artificially treated by dipping in water solution of fenitrothion EC, chlorpyrifos EC and phenthoate EC. The treated apples were washed by the ultrasonic cleaner with water, 30% ethanol solution or 0.2% detergent solution, respectively. The removal efficiency of fenitrothion, chlorpyrifos and phent-hoate by ultrasonicated washing in water for 0.5min. was 39.2%, 32.0% and 50.4%, respectively, but there was a tendency to decrease the removal efficiency of the pesticide residues as the duration of ultrasonicated washing period is increased. The maximum removal efficiency of the pesticide residues washed in the detergent solution was observed by ultrasonicated washing the samples for 5min. and it was recorded as 33.5% ; fenitrothion, 30.1% ; chlorpyrifos and 48.3% ; phenthoate, respectively. However it's appeared that the longer the ultrasonicated washing period in 30% ethanol solution the more pesticides from the apples were removed and the maximum removal efficiency of the pesticides was recorded as 66.2%(fenitrothion ; washed for 15min.), 41.7%(chlorpyrifos ; washed for 10min.), 74.2%(phenthoate ; washed for 10min.).

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Analysis of Residual Solvents of [F-18]FDG Using Gas Chromatography (기체크로마토그래프법을 이용한 [F-18]FDG의 잔류용매 분석)

  • Kim, Dong-Il;Lee, Il-Jung;Kim, Shi-Hwal;Chi, Yong-Gi;Seok, Jae-Dong
    • The Korean Journal of Nuclear Medicine Technology
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    • v.15 no.2
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    • pp.26-29
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    • 2011
  • Purpose: The general test method of the Korean Pharmacopeia specifies the test method on the clauses of quality control after manufacturing. According to KFDA Guidance for Medicines, standards of residual solvents regulates the maximum permissible dose of acetonitrile as 400 ppm, ethanol as 5,000 ppm, and acetic acid as 5,000 ppm. This study aims at identifying the type of resiual solvents in the final [F-18]FDG vial of an automatic synthesizer and measure its residual quantity. Materials and Methods: The center carried out residual solvents test of [F-18]FDG injection using Agilent Technologies 7890A with a Flame Ionization Detector. The column of Agilent Technologies 7890A used in measuring of residual solvents was CP WAX column ($30m{\times}0.53mm{\times}1.0{\mu}m$) and analysis condition was split mode 1:1 at the initial temperature $70^{\circ}C$ which was increased $20^{\circ}C/minute$ after two minutes and maintained at the final $140^{\circ}C$ for two minutes. The analysis method was as following: Firstly, ethanol-acetonitrile-acetic acid mixture was classified into four types of concentration (250-25-250 ppm, 1,000-100-1,000 ppm, 3,000-300-3,000 ppm, and 6,000-600-6,000 ppm), and $1.0{\mu}L$ of each type of concentration was injected into gas chromatography followed by an analysis of its peak domain. Then, a calibration-curve by the external standard method was drawn based on the analysis result. Results: While ethanol and acetonitrile were detected in TRACERlab MX, FASTlab had additional acetic acid. The residual quantity of the ethanol-acetonitrile-acetic acid mixture evaluated using the calibration-curve was average 72 ppm ethanol, 54 ppm acetonitrile, and 1030 ppm acetic acid for FASTlab, whereas average 439 ppm ethanol and 79 ppm acetonitrile for TRACERlab MX. This indicated that both of them were within the maximum permissible dose. Conclusion: Solvent residues in the [F-18]FDG injection were all within maximum permissible doses and proper to be used to examine a patient. The result indicated that types and quantities of solvent resides of radioactive pharmaceuticals vary depending on the automatic synthesizer.

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Use of Accelerated Solvent Extraction Method for Determination of Residual Pesticides in Agricultural Products (농산물의 잔류농약분석을 위한 가속용매추출 (Accelerated Solvent Extraction) 방법의 이용)

  • Lee, Sung-Woo;Seo, Hye-Young;Han, Byung-Jae;Jeong, Yang-Mo;Kim, Jun-Hyoung;No, Ki-Mi;Kim, Kyong-Su
    • Applied Biological Chemistry
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    • v.47 no.2
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    • pp.228-237
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    • 2004
  • ASE (accelerated solvent extraction) was used to develop an analytical method for reducing the sample preparation time in pesticide residues analyses of agricultural produce. The conditions of ASE were as follows: preheat 1 min, heat 5 min, static 1 min, solvent flush% 60 vol., nitrogen purge 60 sec, 4 cycles, 1,500 psi pressure, and $100^{\circ}C$ temperature. When n-hexane:acetone (4 : l, v/v) was used as, an extraction solvent, the extraction and purification efficiency of ASE did not show the considerable difference compared with solvent extraction, and the reduction of extraction solvent did not affect the performance of extraction. It was proved that ASE method can reduce, sample preparation time as the extraction and purification steps were combined, and the extraction solvent was significantly reduced.

Solvent Extraction of Organotin from Ship Wash Wastewater (선박 세척폐수에 함유된 유기주석화합물의 용매추출특성)

  • Song, Young-Chae;Woo, Jung-Hui;Kim, In-Soo;Park, Sang-Ho;Kim, Dong-Geun
    • Journal of Navigation and Port Research
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    • v.28 no.5
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    • pp.463-468
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    • 2004
  • A lab-scale fundamental study to develop the solvent extraction process of ship wash wastewater containing TBT was carried out. For various solvents, including diesels for car and ship, bunker B, thinner, toluene, and ether, the extraction efficiencies of TBT from synthetic ship wash wastewater were compared The effect of extraction conditions, such as solvent amount, time and intensity of agitation, and pH, on the extraction efficiency of TBT was evaluated Diesel for ship showed better extraction efficiency of TBT than those of other tested solvents, and the proper amount of the extraction solvent for 1L of the wastewater was l0mL. When the agitation intensity was increased from 50rpm to 250rpm, the TBT remained in the wastewater after the extraction was decreased from around 120ppb to 2.8ppb. The remaining TBT in the wastewater was sharply decreased from 1hr of the extraction time, but was slightly increased again after 5hrs of the extraction time. The efficiency of TBT extraction was good in the weak acid range of pH, but was not significant as much as the others.

Analysis of Residual Organic Solvent in Environmentally-friendly Farming Materials with Headspace Method (Headspace 법을 사용한 유기농업자재 중 잔류 유기용매 분석)

  • Choi, Geun Hyoung;Kong, Seung-Heon;Park, Byung-Jun;Moon, Byeong-Cheol;Kim, Jin-Hyo
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.128-132
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    • 2016
  • Volatile organic solvents are used to extract the bioactive materials from raw materials for environmentally-friendly farming materials (EFFM), but the solvent should not remain in EFFM for the safety reasons. Thus qualitative and quantitative analysis method for the solvents using Headspace-GC were evaluated. Water content depleted the detection ratio of hydrophilic solvents and disturbing the hydrophilic interaction with solvents by DMSO might be helped to increase the detection ratio (up to 715%). Surfactant concentration affected to the detection ratio (68.5-179.1%) while surfactant type was not deeply involved the solvent detection. On the other hand, matrix-matched calibration method was accepted the minimum requirements for the quantitative analysis of the solvents in EFFM.