• Title/Summary/Keyword: Capillary method

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Quantitative Determination of the Marker Components in Pyungwi-San Using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 평위산 주요 성분의 함량 분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.49 no.3
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    • pp.270-277
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    • 2018
  • Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

Simultaneous Determination of Haloperidol and Its Metabolite, Reduced Haloperidol, in Plasma by Gas Chromatography Using Nitrogen Phosphorous Selective Detection (Gas Chromatography-Nitrogen Phosphorous Selective Detection을 이용한 혈장중 Haloperidol 및 대사체인 Reduced Haloperidol의 동시정량)

  • Park, Kyoung-Ho;Lee, Min-Hwa;Shim, Chang-Koo;Lee, Myung-Gull;Park, Jong-Sei
    • Journal of Pharmaceutical Investigation
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    • v.22 no.3
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    • pp.197-204
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    • 1992
  • A gas chromatographic method using nitrogen phosphorous selective detection was developed for simultaneous determination of haloperidol and its metabolite, reduced haloperidol, in human plasma. Combelen was used as internal standard, The method involved extraction and trimethylsilylation followed by the injection of $2-4\;{\mu}l$ of benzene layer, which was used to dissolve the trimethylsilylated derivatives of haloperidol and reduced haloperidol, onto SE-54 column [5% phenyl methyl silica fused capillary column, $16m{\times}0.22\;mm$ $(I.D.){\times}0.33\;{\mu}m$ (coated thickness)]. The temperature of column oven was programmed from $200^{\circ}C\;to\;300^{\circ}C$ at the increase rate of $10^{\circ}C/min and also the temperatures of injector and detector were set at $300^{\circ}C$. Helium was used as carrier gas and its flow rate was maintained at 30 ml/min. The detection was conducted with nitrogen phosphorous selective detector. The retention times for combelen, reduced haloperidol and haloperidol were found to be 9.14, 9.75 and 9.99 min, respectively. The detection limits for haloperidol and reduced haloperidol in human plasma were both 0.2 ng/ml. The coefficients of variation of the intra-assay were generally low (below 9.8%). The mean absolute recoveries of added haloperidol and reduced haloperidol from plasma were 72% and 84%, respectively. No interferences from endogenous substances were found.

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Some Ultrastructural Observations of the Secretory Processes in Rat Adrenal Medullary Aminergic Cells by TAGO Method (흰쥐 부신수질 아민성세포의 분비과정에 관한 전자현미경적 관찰)

  • Rhyu, Im-Joo;Uhm, Chang-Sub;Suh, Young-Suk
    • Applied Microscopy
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    • v.22 no.1
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    • pp.33-41
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    • 1992
  • To clarify the exocytotic features in adrenal medullary aminergic cells, the authors observed rat adrenal medulla prepared by the TAGO method with transmission electron microscope. Rat adrenal medulla contains two types of aminergic cells, adrenergic and noradrenergic, as described. They were present as a group. In a single group both adrenergic and noradrenergic cells were present, but the same kind of cells showed the tendency forming small groups. Adrenergic cells were characterized with the granules having relatively electroluscent cores. These granules were relatively uniform in size, and the cores filled the granules with only thin halos. Noradrenergic cells were characterized with the granules of various size and forms. Most of the cores of these granules were generally more electron-dense than those of the adrenergic cells and only partly filled the granules without forming the halos. But, some granules were very similar in the shape and electron density as those of the adrenergic cells. Even empty-looking granules were present. Exocytotic figures with the classical omega figures were observed in both types of aminergic cells, but they were more frequent in adrenergic cells. These figures were mainly present along the plasma membranes toward the capillary. The excreted materials could be identified in the cleft of the omega figures. Apocrine-like secretory patterns but without cytoplasmic rims were identified in noradrenergic cells. Some vesicles, possibly formed from the cytoplsmic tubular systems were released. Some irregular lamellar structures of varying sizes were also observed. They looked like membranous structures sneaking through the plasma membranes. We could not, however, found any evidences of their involvement in exocytotic processes. These were present toward the capillaries and found only in the adrenergic cells. The authors conclude that the secretory processes in adrenal chromaffin cells may include not only the classical exocytotic processes but also the unusual direct secretions of granules or parts of cellular organelles. The membranous lamellar structures may indicate the remnants of excreted granules or functionally inactive excess membranes of the organelles removed from the cytoplasm.

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Studies on the Simultaneous Determination of VNA and TSNA by GC - TEA (Gas chromatography-Thermal Energy Analyzer에 의한 휘발성 니트로소아민과 담배 특유의 니트로소아민들의 동시 분석연구)

  • Rhee, Mun-Su;Ji, Sang-Woon;Park, Yang-Su
    • Journal of the Korean Society of Tobacco Science
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    • v.15 no.2
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    • pp.174-184
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    • 1993
  • This is to investigate the methodology for the simultaneous determination of Wk, mk and TSNA using gas chromatography(GC) in combination with chemiluminescence detector, thermal energy analyzer(TEA) . The simultaneous analysis has been estimated by evaluating tobacco. The TEA was linked to GC equipped with non -polar SPB -5 fused silica capillary column which was introduced into the ceramic pyrolysis tube by the point of 16cm from the end of TEA. Quantification was carried out by internal standardization with WDPA after calibration of retention times and response factors with authentic nitrosoamines. It was demonstrated that WDPA was most preferable as internal standard for the simultaneous analysis. The recoveries of the internal standard were in the range of 83∼96% . Nitrosoamines in this method were detected with determination limit of 0.1ng and was made by a straight line in calibration curve by TEA response. The suitability of nitrosoamines extraction in tobacco leaf was investigated. It was most suitable to extract nitrosoamines from tobacco leaves with 0.01 M NaOH within a period of 8 hours. Thimerosal as an antibacterial agent was added to NaOH solution to prevent artifactual formation. The fractionation and the purification of nitrosoamines form alkaline extracts were conveniently performed using Extrelut multilayer column and dichloromethane. Reproducible and reliable results were obtained for the determination of nitrosamines in a relatively short time compared to previous known method. TSNA contents in burley were about 4 times higher as those in the fluecured tobacco.

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Effect of Curvature Dependency of Surface Tension on the Result of Pore-Volume Distribution Analysis (동공부피 분포의 계산결과에 미치는 표면장력의 곡률 의존도 효과)

  • Cho Chang-Hyun;Ahn Woon-Sun;Chang Seihun
    • Journal of the Korean Chemical Society
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    • v.16 no.6
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    • pp.341-348
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    • 1972
  • The significance of the curvature dependency correction of surface tension is studied in calculating the pore volume distribution of porous adsorbent from nitrogen adsorption isotherm. That is, Kelvin radii are calculated with curvature dependent surface tension values calculated by Chang et al, and then with these Kelvin radii, pore volume distributions of three porous adsorbents, silica alumina (steam deactivated), silica gel (Davidson 59), and silica gel (Mallinc-krodt Standard Luminescent), are calculated. The results are compared with those obtained by the previous method in which surface tension is taken as constant and also with the others. obtained by the modelless method proposed by Brunauer et al. The maximum point of the distribution curve shift to the larger pore radius, when the curvature dependency is considered. Furthermore, the relative pressure at which capillary condensation commences is by far the lower than that accepted previously. This effect becomes significant as the pore radius approaches to the micropore range.

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Genetic Relationship of Mono-cotyledonous Model Plant by Ionizing Irradiation (단자엽 모델 식물의 방사선원 별 처리에 따른 유전적 다형성 분석)

  • Song, Mira;Kim, Sun-Hee;Jang, Duk-Soo;Kang, Si-Yong;Kim, Jin-Baek;Kim, Sang Hoon;Ha, Bo-Keun;Kim, Dong Sub
    • Journal of Radiation Industry
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    • v.6 no.1
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    • pp.23-29
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    • 2012
  • In this study, we investigated the genetic variation in the general of monocot model plant (rice) in response to various ionizing irradiations including gamma-ray, ion beam and cosmic-ray. The non-irradiated and three irradiated (200 Gy of gamma-ray and 40 Gy of ion beam and cosmic-ray) plants were analyzed by AFLP technique using capillary electrophoresis with ABI3130xl genetic analyzer. The 29 primer combinations tested produced polymorphism results showing a total of 2,238 bands with fragments sizes ranged from 30 bp to 600 bp. The number of polymorphism generated by each primer combinations was varied significantly, ranging from 2 (M-CAC/E-ACG) to 158 (M-CAT/E-AGG) with an average of 77 bands. Polymorphic peaks were detected as 1,269 with an average of 44 per primer combinations. By UPGMA (Unweighted Pair Group Method using Arithmetic clustering) analysis method, the clusters were divided into non-irradiated sample and three irradiated samples at a similarity coefficient of 0.41 and three irradiation samples was subdivided into cosmic-ray and two irradiation samples (200 Gy of gamma-ray and 40 Gy of ion beam) at similarity coefficient of 0.48. Similarity coefficient values ranged from 0.41 to 0.55.

Permeability of a Capsaicin Derivative $[{14}^C]DA-5018$ to Blood-Brain Barrier Corrected with HPLC Method

  • Kang, Young-Sook;Kim, Jong-Mi
    • Archives of Pharmacal Research
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    • v.22 no.2
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    • pp.165-172
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    • 1999
  • In the present work , the transport mechanism of a capsaicin derivative, DA-5018, through blood-brain barrier (BBB) has been investigated to evaluate the feasibility of potential drug development. The result of pharmacokinetic parameters obtained from the intravenous injection of plasma volume marker,$[3^H]RSA$ and $[{14}^C]DA-5018$, indicated that both AUC, area under the plasma concentration curve and VD, volume of distribution in brain of $[3^H]RSA$ agreed with those reported ($1620{\pm}10 $percentage injected dose minute per milliliter (%IDmin/ml) and $12.0{\pm}0.1{\mu}l/g$, respectively). Elimination half-life and AUC of $[{14}^C]DA-5018$is corrected by the PHLC analysis, 19.6$\pm$1.2 min and 7.69$\pm$0.85% IDmin/ml, respectively. The metabolic rate of $[{14}^C]DA-5018$was very rapid. The blood-brain barrier permeability surface area (PS) product of $[{14}^C]DA-5018$ was calculated to be 0.24$\pm$0.05 $\mu$l/min/g. The result of internal carotid artery perfusion and capillary depletion suggested that [14C]DA-5018 pass through BBB with the time increasingly. Investigation of transport mechanism of $[{14}^C]DA-5018$ using agonist and antagonist suggested that vanilloid (capsaicin) receptor did not exist in the BBB, and nutrient carrier system in the BBB has no effect on the transport of DA-5018. In conclusion, despite the fact that penetration of DA-5018 through BBB is significant, the intact drug found in the brain tissue is small because of a rapid metabolism. Therefore, for the central analgesic effect of DA-5018, the method to increase the metabolic stability in plasma and the brain permeability should be considered.

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Numerical simulation of electrokinetic dissipation caused by elastic waves in reservoir rocks

  • Zhang, Xiaoqian;Wang, Qifei;Li, Chengwu;Sun, Xiaoqi;Yan, Zheng;Nie, Yao
    • Geomechanics and Engineering
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    • v.19 no.1
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    • pp.11-20
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    • 2019
  • The use of electrokinetic dissipation method to study the fluid flow law in micro-pores is of great significance to reservoir rock microfluidics. In this paper, the micro-capillary theory was combined with the coupling model of the seepage field and the current field under the excitation of the harmonic signal, and the coupling theory of the electrokinetic effect under the first-order approximation condition was derived. The dissipation equation of electrokinetic dissipation and viscous resistance dissipation and its solution were established by using Green's function method. The physical and mathematical models for the electrokinetic dissipation of reservoir rocks were constructed. The microscopic mechanism of the electrokinetic dissipation of reservoir rock were theoretically clarified. The influencing factors of the electrokinetic dissipation frequency of the reservoir rock were analyzed quantitatively. The results show that the electrokinetic effect transforms the fluid flow profile in the pores of the reservoir from parabolic to wavy; under low-frequency conditions, the apparent viscosity coefficient is greater that one and is basically unchanged. The apparent viscosity coefficient gradually approaches 1 as the frequency increases further. The viscous resistance dissipation is two orders of magnitude higher than the electrokinetic effect dissipation. When the concentration of the electrolyte exceeds 0.1mol/L, the electrokinetic dissipation can be neglected, while for the electrolyte solution (<$10^{-2}M$) in low concentration, the electrokinetic dissipation is very significant and cannot be ignored.

Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor 및 Trifluralin의 동시 분석)

  • Ahn, Kyung Geun;Kim, Gi Ppeum;Hwang, Young Sun;Kang, In Kyu;Lee, Young Deuk;Choung, Myoung Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.104-116
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    • 2018
  • BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.

A acupuncture therapy literature study on the hemorrhoids and hemorrhoids complicated by anal fistula (치창(痔瘡)과 치루(痔漏)에 대한 침구학적(鍼灸學的) 문헌고찰(文獻考察))

  • Song, Won-sub;Lee, Byung-ryul;Lee, Hyun;Chae, Sang-jin
    • Journal of Acupuncture Research
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    • v.20 no.1
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    • pp.131-143
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    • 2003
  • Objective : The purpose of this study is to arrange the literature about acupuncture therapy on the hemorrhoids and hemorrhoid complicated by anal fistula. Methods : We arrange Huang Di Nei Jing and fifteen kinds of literature about the hemorrhoids and hemorrhoid complicated by anal fistula. Results : 1. The cause of hemorrhoids are overfatigue, overeating, imbalance of stool(const-ipation or diarrhea), uncontrol sexual excess or abstinence, pathgenic factors of wetness, heat, wind, dry, fire, chronical hemorrhoids that has not been treated, and general weakness. 2. Symptom of hemorrhoids is that skin is projected form the nine holes or varicose extension to become hemorrhoid. Hemorrhoids is small nodosity that projected on the anal inter or outer region, and hemorrhoid complicated by anal fistula is pus which comes out form one or some fistula on the anal around inter and outer region. 3. Therapy method of hemorrhoid and hemorrhoid complicated by anal fistula are elimination pathological heat from blood, promote blood flow to remove blood stasis, cold in nature and purge away fire, remove heat form the blood, promote blood flow to remove blood stasis, cold in nature and purge away fire, remove heat from the blood and eliminate dampness, tonify the spleen and replenish Ki, dispel wind and alleviate pain and so forth. Therapy method of hemorrhoid is to give the first consideration to relieve blood: eliminating pathological heat form blood complicated by anal fistula is to tonify the blood first, than after that eliminating pathological heat form blood. About external method are method of fumigation, method of ointment, method of close with medicine, necrotizing method and also operation(injection, bind etc.)was used for treatment. 4. The prescription are Gurgak-hwan, Wypi-hwan, Gunggyi-tang, Jingyochangchul-tang, Jingyobangpung-tang, Mokhyangbinrang-hwan, Ochi-san, Gamihyanso-san, Jojang-hwan, Sinyung-hwan used frequently. 5. food taboo on patient's diet of the hemorrhoid and hemorrhoid complicated by anal fistula are raw grain, cold or dampness food, alcohol, hot food, Singiberis rhizoma recens, Cinnamomi ramulus. 6. Acupuncture therapy on the hemorrhoid and hemorrhoid complicated by anal fistula are, in the first stage eliminating pathological heat form blood and eliminate dampness, and in the long term eliminate dampness, promote and remove meridian energy, remove that form the intestines, dispel channels and collaterals. 7. Acupuncture points at B2, CV1, B58, B36, B56, Sp5, S30, B25, B54, GV1, GV20, L6, B40 used frequently for the acupuncture therapy, and acupuncture point at GV4, GV1, B30, hemorrhoidal point used form moxibustion. Reduction blood at B40 and blue capillary of Sp9 and acupuncture Chungbaek, Ki-gack, Ki-jung, Ki-mun(Dongsh Kihyel) makes the treatment very effective.

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