• 제목/요약/키워드: methyl ether

검색결과 431건 처리시간 0.031초

A Sensitive, Efficient, and Cost-Effective Method to Determine Rotigotine in Rat Plasma Using Liquid-Liquid Extraction (LLE) and LC-MRM

  • Kim, Ji Seong;Jang, Yong Jin;Kim, Jin Hee;Kim, Jin Hwan;Seo, Jae Hee;Park, Il-Ho;Kang, Myung Joo;Choi, Yong Seok
    • Mass Spectrometry Letters
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    • 제13권4호
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    • pp.146-151
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    • 2022
  • Rotigotine (RTG) is a non-ergot dopamine agonist used to manage the early stage of Parkinson's disease (PD) as transdermal patch. However, the poor medication compliance of PD patients and skin issues related with repeated applications of RTG patches lead to the search for alternative formulations and it also requires appropriate analytical methods for their in vivo evaluation. Thus, here, a sensitive, efficient, and cost-effective method to determine RTG in rat plasma using liquid-liquid extraction (LLE) and multiple reaction monitoring was developed. The use of 20 µL of rat plasma for sample treatment, 8-OH-DPAT as the internal standard, and methyl tert-butyl ether as the LLE solvent in the present method gives it advantages over previous methods for the analysis of RTG in biological samples. The good analytical performance of the developed method was confirmed in specificity, linearity (the coefficient of determination ≥0.999 within 0.1-100 ng/mL), sensitivity (the lower limit of quantitation at 0.1 ng/mL), accuracy (81.00-115.05%), precision (≤10.75%), and recovery (81.00-104.48%) by following the FDA guidelines. Finally, the applicability test of the validated method to the in vivo evaluation of a RTG formulation showed that the present method is the only method which can be accurately applied to that longer than 24 hours, critical for the development of formulations with reduced dosing frequencies. Therefore, the present method could contribute to the development of new RTG formulations helpful to people suffering from PD.

Fabrication of Disposable Light Exposure Detector Kit using UV Curable Hydrogels (자외선 경화 하이드로겔을 사용한 일회용 빛 노출 검출 키트의 제조와 특성분석)

  • Kim, Young Ho;Kim, Gyu-Man;Dang, Trung Dung;Choi, Jin Ho;Kim, Hwan-Gon;Park, Sangju;Lee, Sang Hak
    • Applied Chemistry
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    • 제15권1호
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    • pp.17-20
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    • 2011
  • A disposable light exposure detector kit has been developed by UV curing of a hydrogel material. The devised light exposure detector kit consisted of light sensitive structures, bottom plate, character sheet and sticky back plate. A light exposure detector kit has a serial light sensitive structures that contain various light sensitive dyes such as rhodamine and fluorescein. The light sensitive structure composed of UV curable hydrogel polymer material as a supporing material and photosensitive dye in a certain concentration. The fabrication procedure of the ligh exposure detector kit is very simple and fast due to UV curing procedure of a photopolymerizable hydrogel material such as poly(ethylene glycol) methyl ether acrylate (PEGMEA) and poly(ethylene glycol) diacrylate (PEGDA) with a photosensitive dye. By the proposed fabrication method, various size and shape of a light exposure detector kit could be fabricated using a flexible elastomer mold. Due to a fast and inexpensive fabrication method, the light exposure detector kit could be use a single use for various industrial applications. According to light irradation, the light sensitive structure on a light exposure detector kit could be lose its color by decomposition of a photosensitive dye chemical in the structure. Thus the amount of the exposed light on a substrate could easily be recognised by changing color or transparency of the structure.

Removal of Methyl tert-Butyl Ether (MTBE) by Modified Fenton Process for in-situ Remediation (Methyl tert-Butyl Ether(MTBE)의 in-situ Remediation을 위한 Modified Fenton Process에 관한 연구)

  • Chung, Young-Wook;Seo, Seung-Won;Kim, Min-Kyoung;Lee, Jong-Yeol;Kong, Sung-Ho
    • Journal of Soil and Groundwater Environment
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    • 제12권2호
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    • pp.27-36
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    • 2007
  • A recent study showed that MTBE can be degraded by Fenton's Reagent (FR). The treatment of MTBE with FR, however, has a definite limitation of extremely low pH requirement (optimum pH $3{\sim}4$) that makes the process impracticable under neutral pH condition on which the ferrous ion precipitate forming salt with hydroxyl anion, which result in the diminishment of the Fenton reaction and incompatible with biological treatment. Consequently, this process using only FR is not suitable for in-situ remediation of MTBE. In order to overcome this limitation, modified Fenton process using NTA, oxalate, and acetate as chelating reagents was introduced into this study. Modified Fenton reaction, available at near neutral pH, has been researched for the purpose of obtaining high performance of oxidation efficiency with stabilized ferrous or ferric ion by chelating agent. In the MTBE degradation experiment with modified Fenton reaction, it was observed that this reaction was influenced by some factors such as concentrations of ferric ion, hydrogen peroxide, and each chelating agent and pH. Six potential chelators including oxalate, succinate, acetate, citrate, NTA, and EDTA were tested to identify an appropriate chelator. Among them, oxalate, acetate, and NTA were selected based on their remediation efficiency and biodegradability of each chelator. Using NTA, the best result was obtained, showing more than 99.9% of MTBE degradation after 30 min at pH 7; the initial concentration of hydrogen peroxide, NTA, and ferric ion were 1470 mM, 6 mM, and 2 mM, respectively. Under the same experimental condition, the removal of MTBE using oxalate and acetate were 91.3% and 75.8%, respectively. Optimum concentration of iron ion were 3 mM using oxalate which showed the greatest removal efficiency. In case of acetate, $[MTBE]_0$ decreased gradually when concentration of iron ion increased above 5 mM. In this research, it was showed that modified Fenton reaction is proper for in-situ remediation of MTBE with great efficiency and the application of chelatimg agents, such as NTA, was able to make the ferric ion stable even at near neutral pH. In consequence, the outcomes of this study clearly showed that the modified Fenton process successfully coped with the limitation of the low pH requirement. Furthermore, the introduction of low molecular weight organic acids makes the process more available since these compounds have distinguishable biodegradability and it may be able to use natural iron mineral as catalyst for in situ remediation, so as to produce hydroxyl radical without the additional injection of ferric ion.

Determination of finasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 finasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • 제24권5호
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    • pp.345-351
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    • 2011
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

Analysis of dutasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 dutasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Jung, Ki-Kyung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • 제25권1호
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    • pp.76-82
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    • 2012
  • The determination and confirmation of dutasteride in human serum was performed by a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Beclomethasone as an internal standard (I.S.) was added to the serum and the mixed sample was pretreated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE). The mass transitions of dutasteride and I.S. monitored in multiple reaction monitoring (MRM) were m/z 529.6${\rightarrow}$461.5 and m/z 409.3${\rightarrow}$391.2, respectively, and the retention times were 6.45 and 5.46 min, respectively. The calibration curve was linear in the concentration range of 0.5~30.0 ng/mL ($R^2$= 0.9999) and the limit of quantitation (LOQ) was found to be 0.5 ng/mL. The recovery of dutasteride was shown to be 66~72%. The intra-day assay precision and accuracy were in the range 3.5~5.5% and 85.7~89.9%, respectively, and the interday assay precision and accuracy were in the range 4.2~5.8% and 90.8~95.8%, respectively.

Characteristics of Flue Gas Using Direct Combustion of VOC and Ammonia (휘발성 유기 화합물 및 암모니아 직접 연소를 통한 배기가스 특성)

  • Kim, JongSu;Choi, SeukCheun;Jeong, SooHwa;Mock, ChinSung;Kim, DooBoem
    • Clean Technology
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    • 제28권2호
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    • pp.131-137
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    • 2022
  • The semiconductor process currently emits various by-products and unused gases. Emissions containing pollutants are generally classified into categories such as organic, acid, alkali, thermal, and cabinet exhaust. They are discharged after treatment in an atmospheric prevention facility suitable for each exhaust type. The main components of organic exhaust are volatile organic compounds (VOC), which is a generic term for oxygen-containing hydrocarbons, sulfur-containing hydrocarbons, and volatile hydrocarbons, while the main components of alkali exhaust include ammonia and tetramethylammonium hydroxide. The purpose of this study was to determine the combustion characteristics and analyze the NOX reduction rate by maintaining a direct combustion and temperature to process organic and alkaline exhaust gases simultaneously. Acetone, isopropyl alcohol (IPA), and propylene glycol methyl ether acetate (PGMEA) were used as VOCs and ammonia was used as an alkali exhaust material. Independent and VOC-ammonia mixture combustion tests were conducted for each material. The combustion tests for the VOCs confirmed that complete combustion occurred at an equivalence ratio of 1.4. In the ammonia combustion test, the NOX concentration decreased at a lower equivalence ratio. In the co-combustion of VOC and ammonia, NO was dominant in the NOX emission while NO2 was detected at approximately 10 ppm. Overall, the concentration of nitrogen oxide decreased due to the activation of the oxidation reaction as the reaction temperature increased. On the other hand, the concentration of carbon dioxide increased. Flameless combustion with an electric heat source achieved successful combustion of VOC and ammonia. This technology is expected to have advantages in cost and compactness compared to existing organic and alkaline treatment systems applied separately.

Phytochemical Analysis and Anti-cancer Investigation of Boswellia Serrata Bioactive Constituents In Vitro

  • Ahmed, Hanaa H;Abd-Rabou, Ahmed A;Hassan, Amal Z;Kotob, Soheir E
    • Asian Pacific Journal of Cancer Prevention
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    • 제16권16호
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    • pp.7179-7188
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    • 2015
  • Cancer is a major health obstacle around the world, with hepatocellular carcinoma (HCC) and colorectal cancer (CRC) as major causes of morbidity and mortality. Nowadays, there isgrowing interest in the therapeutic use of natural products for HCC and CRC, owing to the anticancer activity of their bioactive constituents. Boswellia serrata oleo gum resin has long been used in Ayurvedic and traditional Chinese medicine to alleviate a variety of health problems such as inflammatory and arthritic diseases. The current study aimed to identify and explore the in vitro anticancer effect of B. Serrata bioactive constituents on HepG2 and HCT 116 cell lines. Phytochemical analysis of volatile oils of B. Serrata oleo gum resin was carried out using gas chromatography-mass spectrometry (GC/MS). Oleo-gum-resin of B. Serrata was then successively extracted with petroleum ether (extract 1) and methanol (extract 2). Gas-liquid chromatography (GLC) analysis of the lipoidal matter was also performed. In addition, a methanol extract of B. Serrata oleo gum resin was phytochemically studied using column chromatography (CC) and thin layer chromatography (TLC) to obtain four fractions (I, II, III and IV). Sephadex columns were used to isolate ${\beta}$-boswellic acid and identification of the pure compound was done using UV, mass spectra, $^1H$ NMR and $^{13}C$ NMR analysis. Total extracts, fractions and volatile oils of B. Serrata oleo-gum resin were subsequently applied to HCC cells (HepG2 cell line) and CRC cells (HCT 116 cell line) to assess their cytotoxic effects. GLC analysis of the lipoidal matter resulted in identification of tricosane (75.32%) as a major compound with the presence of cholesterol, stigmasterol and ${\beta}$-sitosterol. Twenty two fatty acids were identified of which saturated fatty acids represented 25.6% and unsaturated fatty acids 74.4% of the total saponifiable fraction. GC/MS analysis of three chromatographic fractions (I,II and III) of B. Serrata oleo gum resin revealed the presence of pent-2-ene-1,4-dione, 2-methyl- levulinic acid methyl ester, 3,5- dimethyl- 1-hexane, methyl-1-methylpentadecanoate, 1,1- dimethoxy cyclohexane, 1-methoxy-4-(1-propenyl)benzene and 17a-hydroxy-17a-cyano, preg-4-en-3-one. GC/MS analysis of volatile oils of B. Serrata oleo gum resin revealed the presence of sabinene (19.11%), terpinen-4-ol (14.64%) and terpinyl acetate (13.01%) as major constituents. The anti-cancer effect of two extracts (1 and 2) and four fractions (I, II, III and IV) as well as volatile oils of B. Serrata oleo gum resin on HepG2 and HCT 116 cell lines was investigated using SRB assay. Regarding HepG2 cell line, extracts 1 and 2 elicited the most pronounced cytotoxic activity with $IC_{50}$ values equal 1.58 and $5.82{\mu}g/mL$ at 48 h, respectively which were comparable to doxorubicin with an $IC_{50}$ equal $4.68{\mu}g/mL$ at 48 h. With respect to HCT 116 cells, extracts 1 and 2 exhibited the most obvious cytotoxic effect; with $IC_{50}$ values equal 0.12 and $6.59{\mu}g/mL$ at 48 h, respectively which were comparable to 5-fluorouracil with an $IC_{50}$ equal $3.43{\mu}g/mL$ at 48 h. In conclusion, total extracts, fractions and volatile oils of B. Serrata oleo gum resin proved their usefulness as cytotoxic mediators against HepG2 and HCT 116 cell lines with different potentiality (extracts > fractions > volatile oil). In the two studied cell lines the cytotoxic acivity of each of extract 1 and 2 was comparable to doxorubicin and 5-fluorouracil, respectively. Extensive in vivo research is warranted to explore the precise molecular mechanisms of these bioactive natural products in cytotoxicity against HCC and CRC cells.

Simultaneous Determination of Cholesterol, Bile Acids and Sterols in Human Bile Juices and Gallstones Using GC/MS (GC/MS에 의한 담석과 담즙내의 Cholesterol, Bile Acids 및 Sterols의 동시 Profiling)

  • Yang, Yoon Jung;Lee, Seon Hwa;Kim, Hyun Joo;Chung, Bong Chul
    • Journal of the Korean Chemical Society
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    • 제42권3호
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    • pp.266-276
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    • 1998
  • Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

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Synthesis and Property of Modified PMMA Resin Using Polyurethane and Polyurethane Dimethacrylate (Polyurethane과 polyurethane dimethacrylate를 이용한 내충격성 PMMA수지의 합성과 그 물성)

  • Kim, Dong-Hyun;Kim, Ju-Young;Seo, Kyung-Do
    • Applied Chemistry for Engineering
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    • 제4권3호
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    • pp.616-626
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    • 1993
  • Polyurethane(PU) have an excellent flexibility and toughness so that it has been widely used as an elastomer. PMMA was blended with PU to improve the impact property. Five types of PU, having different molecular weight and different polyol types, were prepared and blended with PMMA in order to investigate the effect of molecular weight and polyol type of PU on property of PU-PMMA blend. Tensile strength of PU-PMMA blend was determined by Inston. Differential Scanning Calorymetry(DSC) and Scanning. Elctron Microscopy(SEM) were used to observe morphology change and glass transition temperature changes of PU-PMMA blends. Transparency of PU-PMMA blends was determined by haze meter. But, owing to intrinsic incompatability of PU-PMMA, Low impact strength of PMMA wasn't improved through PU-PMMA blend. therefore, polyurethane dimethacrylate(PUD), having similiar chemical structure to PU and two vinyl group at both ends, was prepared and reacted with methyl methacrylate(MMA) to form crosslinked copolymer Mechanical property of this crosslinked polymer, such as impact strength and transparency, was investigated by Instron, Izod type (Cantilever beam) impact tester and haze meter. Results of these measurements showed that crosslinked copolymer of PUD-MMA was better impact resistance than PMMA and maintained similar transparency to PMMA.

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Extension of Low Temperature Combustion Regime by Turbocharging Using Diesel and Biodiesel Fuels (과급에 의한 디젤 및 바이오디젤의 저온연소 운전영역 확장에 관한 연구)

  • Jang, Jae-Hoon;Oh, Seung-Mook;Lee, Yong-Gyu;Lee, Sun-Youp
    • Transactions of the Korean Society of Mechanical Engineers B
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    • 제36권11호
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    • pp.1065-1072
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    • 2012
  • Due to its oxygen (O) content, biodiesel (BD) is advantageous in that it lowers PM emissions in CI engines. Therefore, BD is considered one of the best candidates for low temperature combustion (LTC) operation because its use can extend the regime for simultaneous reduction of PM and $NO_x$. Thus, in this study, LTC operation was realized using BD and diesel with a 5~7% $O_2$ fraction. Engine test results show that the use of BD increased the efficiency and reduced emissions such as PM, THC, and CO; furthermore, IMEP reduced by 10~12% owing to the lower LHV of the fuel. In particular, smoke was suppressed by up to 90% because O atoms in the BD enhanced the soot oxidation reaction. To compensate the IMEP loss, turbocharging (TC) was then tested, and the results showed that the power output increased and PM was reduced further. Moreover, TC in BD engine operation allowed a similar level of reduction in both $NO_x$ and PM at 11~12% $O_2$ fraction, suggesting that there is a potential to widen the operating range by the combination of TC and BD.