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.
A polypropylene fraction collected from the stream of post-consumer plastics was pyrolyzed. The aim of this study is to observe the dependence of yield of BTEX-aromatics normally used as solvent on the reaction temperature. To reach the goal, three experiments were carried out at different temperature between 650 and $700^{\circ}C$, using a fluidized bed reactor that shows an excellent heat transfer. In the experiments, product gases were used as a fluidizing medium to maximize the amount of BTEX-aromatics at fixed flow rate and feed rate during the pyrolysis. Oil, gas and char were obtained as product fractions. Product gases were analyzed with GCs(TCD, FID) and with a GC-MS system for qualitative analysis. For an accurate analysis of product oil, the product oil was distilled under vacuum, and separated the distillation residues from oil fractions that were actually analyzed with a GC-MS system. As the reaction temperature went higher, the content of BTEX-aromatics increased. The maximal yield of BTEX-aromatics was obtained at $695^{\circ}C$ with a value of about 30%. The main compounds of product gas were $CH_4$, $C_2H_4$, $C_2H_6$, $C_3H_6$, $C_4H_{10}$ and the product gas had an higher heating value about 45MJ/kg. It could be used as a heat source for a pyrolysis plant or for other fuel applications.
Kaempferia parviflora, an herbaceous plant in the family Zingiberaceae, is popular in many tropical regions. It is called as black ginger or krachaidum in Thailand and Laos, and its raw or dried root have been used as spices and teas. The rhizomes also have been traditionally used to treat gastrointestinal disorders, ulcers, gout, dysentery, allergies and to improve physical work capacity. Recently, its anti-obesity, anti-oxidant, anti-inflammatory and blood clot-lysis activities were reported. In this study, the anti-thrombosis activity of black ginger was investigated, since improvement in blood fluidity leads to the prevention of various lifestyle-related diseases. The hot water and ethanol extract and their subsequent solvent fractions (hexane, ethylacetate, butanol fractions and water residue) were prepared, and their anti-coagulation and platelet aggregation inhibitory activities were determined, respectively. Among the black ginger extracts and their fractions, the ethylacetate fraction (EAF) of ethanol extract only showed significant extensions of blood coagulation time determined by thrombin time (TT), prothrombin time (PT), and activated partial thromboplastin time (aPTT). At 5 mg/ml concentration, TT, PT and aPTT were extended to 1.22, 1.49 and >15-folds compared to non-treatment. The EAFs of ethanol and hot water extract showed strong inhibitions against collagen-induced platelet aggregations, which are comparable to inhibitions of aspirin. Also the EAFs from black ginger did not show any hemolysis activity against human RBC up to 0.5 mg/ml. Our results suggest that the EAF of black ginger has a potential as novel anti-coagulation and ant-platelet aggregation agent. This report provides the first evidence of anti-coagulation activity of black ginger.
Kim, Jee-In;Jang, Han-Su;Kim, Jong-Sik;Sohn, Ho-Yong
Microbiology and Biotechnology Letters
/
v.37
no.2
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pp.133-139
/
2009
Yam (Dioscorea batatas Decne) has been recognized as healthy food due to its various biological activities, such as anti-obesity, anti-constipation, anti-proliferation, anti-mutagenic activity, and decrease of blood glucose and cholesterol level. In this study, the methanol extract and its organic solvent fractions were prepared from dried Dioscorea batatas Decne, and their antimicrobial, antithrombin, and antioxidant activity were evaluated, respectively. The 66.7% of methanol extract was fractioned into water residue, and most of total-polyphenol/total-flavonoids were found in ethylacetate fraction. This ethylacetate fraction at $500\;{\mu}g/disc$ concentration showed strong antibacterial activity against gram-negative and gram-positive bacteria, except Staphylococcus aureus. Antifungal activity was not observed in methanol extract and its fractions. But, strong antithrombin activity was found in methanol extract. At 4.8 mg/mL concentration, thrombin time was 99.5 sec, which is coincides with 30% activity of aspirin, a commercial available antithrombosis agent. The ethylacetate fraction showed strong DPPH scavenging activity ($IC_{50}$ of $80.5\;{\mu}g/mL$), compared to vitamin C ($IC_{50}$ of $15.2\;{\mu}g/mL$). Also, the ethylacetate fraction showed strong SOD-like activity and reducing power, which are coincide with 43% of vitamin C and 82.7% of butylated hydroxytoluene activity, respectively.
Thermal behavior of poly (methyl methacrylate) was analyzed in the presence of tin (IV) chloride. Five different proportions - polymer to additive - were selected for casting films from common solvent. TG, DTG and DTA were employed to monitor thermal degradation of the systems. IR and py-GC-MS helped identify the decomposition products. The blends start degrading at a temperature lower than that of the neat polymer and higher than that of the pure additive. Complex formation between tin of additive and carbonyl oxygen (pendent groups of MMA units) was noticed in the films soon after the mixing of the components in the blends. The samples were also heated at three different temperatures to determine the composition of residues left after the expulsion of volatiles. The polymer, blends and additive exhibited a one step, two-step and three-step degradation, respectively. $T_0$ is highest for the polymer, lowest for the additive and is either $60^{\circ}C$ or $70^{\circ}C$ for the blends. The amount of residue increases down the series [moving from blend-1 (minimum additive concentration) to blend-5 (maximum additive concentration)]. For blend-1, it is 7% of the original mass whereas it is 16% for blend-5. $T_{max}$ also goes up as the concentration of additive in the blends is elevated. The complexation appears to be the cause of observed stabilization. Some new products of degradation were noted apart from those reported earlier. These included methanol, isobutyric acid, acid chloride, etc. Molecular-level mixing of the constituents and "positioning effect" of the additive may have brought about the formation of new compounds. Routes are proposed for the appearance of these substances. Horizontal burning tests were also conducted on polymer and blends and the results are discussed. Activation energies and reaction orders were calculated. Activation energy is highest for the polymer, i.e., 138.9 Kcal/mol while the range for blends is from 51 to 39 Kcal/mol. Stability zones are highlighted for the blends. The interaction between the blended parts seems to be chemical in nature.
The black currant (Ribes nigrum L.) is belong to the Grossulariaceae family, and has piquant berries, which can be eaten as raw or as processed foods, such as jams, jelly, juice and syrups. In this study, the fresh juice of black currant (FJBC) from Austria and its subsequent organic solvent fractions, such as hexane fraction, ethylacetate (EA) fraction, butanol fraction and water residue, were prepared and their in-vitro anti-oxidant, anti-coagulation and anti-platelet aggregation activities were evaluated. The FJBC and EA fraction, which has concentrated polyphenol and flavonoid, showed strong radical scavenging activities and reducing power. The $RC_{50}s$ of EA fraction against DPPH anion, ABTS cation, nitrite were 136.3, 66.2 and $115.5{\mu}g/ml$, respectively, those are 1/10, 1/16, and 1/7.7 of $RC_{50}s$ of vitamin C. In anti-coagulation assay, the FJBC, EA and butanol fraction showed significant inhibitory activities against thrombin, prothrombin and coagulation factors. Furthermore, the anti-platelet aggregation activities of EA and butanol fraction were the stronger than that of aspirin. The concentrations required for 50% platelet aggregation inhibition of aspirin, EA and butanol fraction were 0.395, 0.192 and 0.261 mg/ml, respectively. The EA and butanol fraction have no hemolysis activities up to 0.5 mg/ml against human red blood cells. The results suggest that the FJBC and its EA and butanol fraction have high potentials as novel anti-thrombosis agents. This report provides the first evidence of anti-thrombosis activity of black currant.
For this study, we prepared organic solvent fractions from methanol extracts of Houttuynia cordata and Lespedeza cuneate, and analyzed their chemical components and various biological functions such as anti-oxidation, angiotensin-converting enzyme (ACE) inhibition, and α-glucosidase inhibitory activities. We found that DPPH radical scavenging activity was highest in the ethyl acetate fractions of Houttuynia cordata (90.8%) and Lespedeza cuneata (91.2%), whereas ABTS radical scavenging activity was highest in the ethyl acetate fractions of Houttuynia cordata (86.1%) and the chloroform fractions of Lespedeza cuneata (95.6%). FRAP activity was highest in the ethyl acetate fraction of Houttuynia cordata (360.1 mg TE/g) and Lespedeza cuneata (239.2 mg TE/g). ACE inhibitory activity was highest in the chloroform fraction of Houttuynia cordata (13.2%) and Lespedeza cuneata (35.2%). And, α-glucosidase inhibitory activity was highest in the ethyl acetate fraction of Houttuynia cordata (56.3%), and the water residue of Lespedeza cuneata (93.6%). Finally, we investigated the DPPH radical scavenging activity of 20 types of pure compounds identified in Houttuynia cordata and Lespedeza cuneate. The results show that quercetin demonstrates the highest DPPH radical scavenging activity. Overall, these results help us to understand the functional chemical components of Houttuynia cordata and Lespedeza cuneate and the biological effects of these components.
Kim, Eun-Hee;Jang, Mi-Ra;Kim, Jin-A;Kim, Tae-Rang;Yook, Dong-Hyun;Hwang, In-Sook;Kim, Jung-Hun
Korean Journal of Food Science and Technology
/
v.43
no.3
/
pp.277-281
/
2011
A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were $73.6{\mu}g/kg$ and $29.8{\mu}g/kg$.
We propose an effective and environmentally friendly dry stripping method using a supercritical carbon dioxide ($SCCO_2$) system modified by a single and multiple cosolvents to remove ion-implanted photoresist and residue from a wafer surface at three different temperatures (97, 148, $200^{\circ}C$) and pressures (200, 300, 400 bar). After high dose of ion implantation the photoresist was not easily removed by using pure $SCCO_2$, but swollen. The $SCCO_2$ system modified by single cosolvents and multiple cosolvents mixed with aprotic solvents could not effectively remove the heavy organics, but swell them. However, the $SCCO_2$ system modified with multiple cosolvent (5%, v/v) composed of DMSO and DIW showed high removal efficiency for ion-implanted photoresists at $97^{\circ}C$ and 200 bar for 30 min (about 80%). In this study it has been shown that the dry stripping method using $SCCO_2$ system modified with multiple cosolvents could replace either plasma ashing or acid and solvent wet bench method and dramatically reduce accompanied chemical usage and disposal.
The present study was carried out to isolate and identify of antioxidants from makgeolli. Makgeolli (3 L) was filtered and the residue was extracted by MeOH. The combined filtrates and MeOH extracts were successively solventfractionated by n-hexane, EtOAc, and BuOH. In the antioxidative activity against DPPH and $ABTS^+$ radicals of each fraction obtained after solvent-fractionation, EtOAc and BuOH layers showed higher activities than other fractions. Therefore, the two layers were respectively purified by column chromatography and HPLC. The isolated compounds were subjected to NMR and MS analyses and identified as 4-hydroxybenzaldehyde (1, 2.0 mg), 2-(4-hydroxyphenyl)ethanol (2, tyrosol, 15.3 mg), trans- and cis-ferulic acids (3 and 4, 1.2 mg), 1H-indole-3-ethanol (5, tryptophol, 3.4 mg), dimethyl succinate (6, 14.9 mg), succinic acid (7, 7.4 mg), and mono-methyl succinate (8, 7.8 mg). The presence of 1-5 in makgeolli have never before been reported.
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