• 제목/요약/키워드: HPLC analysis methods

검색결과 485건 처리시간 0.031초

Frontal Analysis와 Pulse Input Method를 이용한 Loxoprofen의 등온흡착식 결정 (Determination of Loxoprofen Adsorption Isotherms by Frontal Analysis and Pulse Input Method)

  • 이은;박준섭;김인호
    • KSBB Journal
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    • 제21권5호
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    • pp.371-375
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    • 2006
  • 본 실험의 목적은 frontal analysis(FA)와 pluse input method(PIM) 방법으로 흡착분리공정에 있어서 중요한 전 단계의 하나인 등온흡착식을 결정하는데 있다. FA를 수행하기에 앞서 대상물질이었던 loxoprofen의 용해도를 측정하여 hexane/ethanol=95/5일 때 시료의 농도를 $0.2{\sim}3mg/ml$로 결정하고, pH조정을 위한 acetic acid는 0.5%로 결정하였다. 이동상의 주성분인 hexane의 조성이 증가함에 따라 용해도는 감소하였지만 분리도는 증가하는 경향을 확인하였다. 이런 용해도와 분리도 사이의 trade-off 또한 흡착분리과정에서의 조작변수가 될 수 있음을 의미한다. FA로 구한 이성분계 등온흡착식은 $$C_{S,re}=\frac{5.282C_{M,re}}{1+0.1412C_{M,re}+0.2139C_{M,ex}}$$, $$C_{S,ex}=\frac{6.413C_{M,ex}}{1+0.2139C_{M,ex}+0.1412C_{M,re}}$$로 결정하였고, PIM으로 구한 이성분계 등온흡착식은 $$C_{S,re}=\frac{5.245C_{M,re}}{1+0.1667C_{M,re}+0.2054C_{M,ex}}$$, $$C_{S,ex}=\frac{6.061C_{M,ex}}{1+0.2054C_{M,ex}+0.1667C_{M,re}}$$로 결정 하였다.

Qualitative and quantitative analysis of furosine in fresh and processed ginsengs

  • Li, Yali;Liu, Xiaoxu;Meng, Lulu;Wang, Yingping
    • Journal of Ginseng Research
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    • 제42권1호
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    • pp.21-26
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    • 2018
  • Background: Furosine (${\varepsilon}$-N-2-furoylmethyl-L-lysine, FML) is an amino acid derivative, which is considered to be an important indicator of the extent of damage (deteriorating the quality of amino acid and proteins due to a blockage of lysine and a decrease in the digestibility of proteins) during the early stages of the Maillard reaction. In addition, FML has been proven to be harmful because it is closely related to a variety of diseases such as diabetes. The qualitative analysis of FML in fresh and processed ginsengs was confirmed using HPLC-MS. Methods: An ion-pair reversed-phase LC method was used for the quantitative analysis of FML in various ginseng samples. Results: The contents of FML in the ginseng samples were 3.35-42.28 g/kg protein. The lowest value was observed in the freshly collected ginseng samples, and the highest value was found in the black ginseng concentrate. Heat treatment and honey addition significantly increased the FML content from 3.35 g/kg protein to 42.28 g/kg protein. Conclusion: These results indicate that FML is a promising indicator to estimate the heat treatment degree and honey addition level during the manufacture of ginseng products. The FML content is also an important parameter to identity the quality of ginseng products. In addition, the generation and regulation of potentially harmful Maillard reaction products-FML in ginseng processing was also investigated, providing a solid theoretical foundation and valuable reference for safe ginseng processing.

태음인(太陰人) 청심연자탕(淸心蓮子湯)의 동시분석 및 항비만 효과 (Simultaneous Analysis and Anti-obesity Effect of Taeeumin Cheongsimyeonja-tang)

  • 서창섭;정수진;김정훈;유새롬;신현규
    • 사상체질의학회지
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    • 제25권1호
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    • pp.51-61
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    • 2013
  • Objectives We performed the simultaneous analysis for three compounds in Cheongsimyeonja-tang (CSYJT) and evaluated its anti-obesity effect. Methods The column for separation of three compounds was used Gemini $C_{18}$ column and maintained at $40^{\circ}C$. The mobile phase for gradient elution consisted of two solvent systems. The analysis was carried out at a flow rate of 1.0 mL/min with PDA detection at 275 nm. The injection volume was $10{\mu}L$. 3T3-L1 preadipocytes were differentiated into adipocytes by adding insulin, dexamethasone and 3-isobutyl-1-methylxanthine (IBMX) for 8 days in the absence or presence of CSYJT. Anti-obesity effects of CSYJT were evaluated by Oil Red O staining, glycerol-3-phosphate dehydrogenase (GPDH) activity, triglyceride contents, and leptin production. Results Calibration curves were acquired with $r^2$ >0.9999. The contents of baicalin, wogonoside and baicalein in CSYJT were 14.54-14.65 mg/g, 5.24-5.27 mg/g and 0.01-0.02 mg/g, respectively. CSYJT showed inhibitory effect on lipid accumulation and GPDH activity in the differentiated 3T3-L1 cells. Furthermore, CSYJT significantly decreased contents of triglyceride and leptin production in 3T3-L1 adipocytes. Conclusions These results will be helpful to improve quality control and anti-obesity effect of Taeeumin CSYJT.

Classification of Red Wines by Near Infrared Transflectance Spectroscopy

  • W.Guggenbichler;Huck, C.W.;M.Popp;G.K.Bonn
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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    • pp.1516-1516
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    • 2001
  • During the recent years, wine analysis has played an increasing role due the health benefits of phenolic ingredients in red wine [1]. On the other hand there is the need to be able to distinguish between different wine varieties. Consumers want to know if a wine is an adulterated one or if it is based on the pure grape. Producers need to certificate their wines in order to ensure compliance with legal regulations. Up to now, the attempts to investigate the origin of wines were based on high-performance liquid chromatography (HPLC), gas chromatography (GC) and pyrolysis mass spectrometry (PMS) [l,2,3]. These methods need sample pretreatment, long analysis times and therefore lack of high sample throughput. In contradiction to these techniques using near infrared spectroscopy (NIRS), no sample pretreatment is necessary and the analysis time for one sample is only about 10 seconds. Hence, a near infrared spectroscopic method is presented that allows a fast classification of wine varieties in bottled red wines. For this, the spectra of 50 bottles of Cabernet Sauvignon, Lagrein and Sangiovese (Chianti) were recorded without any sample pretreatment over a wavelength range from 1000 to 2500 nm with a resolution of 12 cm$\^$-1/. 10 scans were used for an average spectrum. In order to yield best reproducibility, wines were thermostated at 23$^{\circ}C$ and a optical layer thickness of 3 mm was used. All recorded spectra were partitioned into a calibration and validation set (70% and 30%). Finally, a 3d scatter plot of the different investigated varieties allowed to distinguish between Cabernet Sauvignon, Lagrein and Sangiovese (Chianti). Considering the short analysis times this NRS-method will be an interesting tool for the quality control of wine verification and also for experienced sommeliers.

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병풀 지상부 조직에서 시기별 triterpene glycoside 함량 및 항산화활성 분석 (Analysis of Triterpene Glycoside Levels and Antioxidant Activity in the Different Shoot Tissues of Centella asiatica (L.) Urban)

  • 길영숙;신승미;이동열;정원민;;이신우;김윤희;구영민
    • 생명과학회지
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    • 제28권8호
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    • pp.917-922
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    • 2018
  • 본 연구에서는 약용식물인 병풀의 계절적 생육조건의 변화에 따른 다양한 지상부 조직에서 triterpene glycoside 함량을 조사하기 위해, 20% 에탄올, 메탄올, 물을 이용한 3가지 추출방법을 이용하여 HPLC 분석을 수행하였다. 메탄올 추출방법에서 triterpene glycoside의 추출효율이 가장 높았으며, 특히 madecassoside와 asiaticoside의 값이 계절적인 생육조건의 변화동안 높게 확인되었다. 본 연구에서는 추가적으로 항산화활성을 분석하였으며, ABTs 소거활성은 잎자루에서 높게 확인되었으며, DPPH 소거활성은 메탄올과 에탄올로 추출한 잎조직에서만 높은 결과를 보였다. 총 페놀 및 플라보노이드 함량은 잎 조직에서 사용된 물, 에탄올, 메탄올 추출에 의한 결과가 가장 높은 값을 보였다. 본 연구의 결과로서, 병풀 식물체의 잎 조직에서 계절적 생육 조건 동안 triterpene glycoside 및 항산화활성이 증가함은 병풀의 재배시 madecassoside 및 asiaticoside를 포함한 유용한 주요 대사물질들이 식물체내에서 항상성을 위해 유지되며, 이는 향후 보 다 구체적인 생리활성에 대한 연구가 필요할 것으로 생각되는 바이다.

남조류로부터 마이크로시스틴을 추출하는 새로운 추출법 연구 (Study on New Extraction Method of Microcystins from Cyanobacteria)

  • 표동진;신현두
    • 대한화학회지
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    • 제45권2호
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    • pp.149-155
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    • 2001
  • 남조류독소, 마이크로시스틴을 초임계유체추출을 이용하여 추출하는 새로운 분석법이 개발되었다. 이 연구에서 사용된 마이크로시스틴들은 초임계 유체 CO$_2$에는 거의 녹지 않지만 90% CO$_2$, 9.0% 메탄올, 1.0% 물로 된 혼합유체를 사용한 결과 성공적으로 추출할 수 있었다. 이 연구에서 사용된 초임계 유체 추출법은 고체상추출법보다 많은 장점들을 가지고 있다. 우선 시료처리단계가 줄어들고, 시료의 손실이 적으며, 분석시간을 단축시킬 수 있다는 장점들이 있다. 또한 전처리 단계가 생략된다는 장점도 있다. ODS 카트리지를 사용하는 고체상 추출법에서 ODS 카트리지가 마이크로시스턴에 대한 흡착력이 떨어지기 때문에 좀 더 극성이 있는 CN 카트리지에 주입시켰다. CN 카트리지는 물 5mL, 0.5 M 아세트산 5mL, 5% 아세트니트릴 5mL로 빗은 후 70% 아세트니릴로 최종용리시킨 후 HPLC로 분리하였다. CN 카트리지를 사용하였을 때 ODS 카트리지보다 더 좋은 회수율과 크로마토그램을 보여주었다.

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감초 중 리퀴리티게닌 분석법 개발 및 함량분석 (Analysis of Liquiritigenin, an Aglycone of Liquiritin in Licorice by High Performance Liquid Chromatography)

  • 이종화;제금련;김도훈;박주영;심영훈;김종환;임숙;신진선;김인선;김지연;성상현;장승엽;김동섭;성락선
    • 생약학회지
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    • 제40권4호
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    • pp.309-314
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    • 2009
  • Licorice(Glycyrrhizae Radix et Rhizoma) is recorded as the root of Glycyrrhiza uralensis Fischer or Glycyrrhiza glabra Linne or Glycyrrhiza inflata Bat.(Leguminosae) in Korean Pharmacopoeia $9^{th}$ edition (KP9) and Chinese Pharmacopoeia 2005(CP2005), Glycyrrhiza uralensis Fischer or Glycyrrhiza glabra Linne in Japanese Pharmacopoeia 2005(JP2005). It is established the content standard of Glycyrrhizin 2.5 % and liquiritin 1% in KP9 and CP2005. But, according to the reports, all Licorice species were not sufficient for content standard of liquiritin 1.0% for licorice in KP9 and CP2005. It shows different content of liquiritin among G. uralensis, G. glabra and G. inflata. Also, it was reported liquiritin, liquiritin apioside are transformed into liquiritigenin by human internal flora. Therefore, we have studied for the pre-treatment condition and analytical method of liquiritigenin; It was good efficinet in 2M HCl reflux(1 hr) for hydrolysis and in methylene chloride for solvent fractionation. And 1% acetic acid in DW(A) and acetonitrile(B) with gradient condition as a mobile phase was most effective in HPLC analytical condition. According to these experimental methods, we have anlayzed content of liquiritigenin about 77 Licorice sample. In this research, it was also examined the content of liquiritin and liquiritigenin for Glycyrrhizae Radix related growing area. According to the results, we suggested the content standard of glycyrrhizin more than 2.5%, liquiritigenin more than 0.7%(after hydrolysis) of licorice.

가열 추출법과 마이크로웨이브 추출법을 이용한 황금 물 추출물의 뇌세포 보호 및 항산화 효과 비교 연구 (The Comparison between Hot-Water Extracts and Microwave Extracts of Scutellaria radix for Antioxidant and Neuroprotective Effects)

  • 이동성;고원민;김경수;김동철;윤치수;조광호;최향;오현철;김윤철
    • 생약학회지
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    • 제45권1호
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    • pp.55-61
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    • 2014
  • Microwaves are non-ionizing electromagnetic waves of frequency between 300MHz to 300GHz and positioned between the X-ray and infrared rays in the electromagnetic spectrum. In recent years, the use of microwave for extraction of ingredient from plant material has shown remarkable research interest and potential. Scutellaria radix has been used as a traditional medicine for a variety of diseases. It has been reported to exert beneficial health effects, such as anti-bacterial, antiviral, anti-inflammatory, and free-radical scavenging. Oxidative stress or the accumulation of reactive oxygen species (ROS) leads neuronal cellular death and dysfunction, and it contributes to neuronal degenerative disease such as Alzheimer's disease, Parkinson's disease and stroke. In this study, we aimed to compare the neuroprotective and antioxidant effect of Scutellaria radix extracted by different methods using hot-water extraction (SBE-DW) or microwave extraction (SBE-DW-MW). As a result, we first examined HPLC analysis of hot-water and microwave extracts of Scutellaria radix. The hot-water and microwave extracts of Scutellaria radix showed the discernible difference patterns of HPLC analysis. Microwave-water extracts of Scutellaria radix increased DPPH radical scavenging activity more than hot-water extraction. Microwave-water extracts of Scutellaria radix also showed neuroprotective effects and ROS inhibition against glutamate-induced oxidative stress in mouse hippocampal HT22 cells, but hot-water extraction not showed. In addition, the phosphorylation of MAPKs induced by glutamate insult was prevented by microwave-water extracts of Scutellaria radix. Thus, these results suggested that microwave extraction can be utilized for improving the extraction efficiency and biological activity of Scutellaria radix.

후박(厚朴)의 외.내부형태 및 이화학패턴연구 (A Study of Morphology and Pattern Analysis in Magnoliae Cortex)

  • 이금산;김정훈;최고야;강대훈;황성연;정승일;김홍준;주영승
    • 대한본초학회지
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    • 제23권4호
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    • pp.21-29
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    • 2008
  • Objectives: To determine the standards for discrimination of Magnoliae Cortex, the experiment of specific external-internal characters and the physicochemical pattern analysis were performed. Methods: External characteristics was observed using a stereoscope. Paraffin-mediated sectioned materials were stained by Ju's method. Physicochemical patterns of materials were analyzed using HPLC. Results: 1. Botanical characteristics: Magnolia officinalis had one seed and a white flower, while M. obovata had two seeds and a white flower. Machilus thunbergii had berry and spherical fruits and yellowish green panicles. 2. External characteristics: M. officinalis and M obovata were dark and thick. M. officinalis was gray brown and greasy while M. obovata was light-gray, less oily and smoothly sectioned. Machilus thunbergii was thin and relatively light or yellow-brown, coarsely sectioned and faintly specific scents. 3. Internal characteristics: The bast parts of M. officinalis and M. obovata were commonly wider than Machilus thunbergii The cork cortex of M. officinalis was $10{\sim}mg/L$ cell layers with many oil cells, while that of M. obovata was $4{\sim}7$ cell layers with less oil cells. Machilus thunbergii's xylem which consisted of ring-shaped cambium at 1st and 2nd part was occupied in large portion. 4. Physicochemical pattern: Both M. officinalis and M. obovata involved honokiol and magnolol. All kinds of M. officinalis involved Magnatriol B but one kind of M. ovobata and all of Machilus thunbergii didn't. Machilus thunbergii showed different pattern of chromatogram from that of 2 species above. Conclusions: These results could be used as standards for discrimination of Magnoliae Cortex and as the method of objectification in medicinal herbs giving the basic resource for bioactivity research.

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소시호탕에서 baicalin과 glycyrrhizin 동시 분석 및 항염 활성 (Simultaneous determination of baicalin and glycyrrhizin in Sosiho-tang by HPLC and anti-inflammatory activity)

  • 김정훈;하혜경;서창섭;이진아;신현규
    • 대한본초학회지
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    • 제26권1호
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    • pp.41-46
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    • 2011
  • Objectives : To quantitate the main compounds and investigate the biological activity of Sosiho-tang (Xiao-Chai-Hu-Tang, SST), simultaneous determination of baicalin and glycyrrhizin, and anti-inflammatory activity were estimated. Methods : A quantitative analysis was performed using a high performance liquid chromatography (HPLC). Reference compounds were separated on a reversed-phase column using gradient elution with water and acetonitrile each containing acetic acid at a flow rate of 1 mL/min. And the productions of nitric oxide (NO) and prostaglandin $(PE)E_2$ were examined by lipopolysaccharide (LPS)-treated RAW 264.7 cells in the presence of the SST. The anti-inflammatory activity of SST was investigated by carrageenin-induced paw edema in rats. The paw volume was measured at 2 and 4 hr following carrageenin-induced paw edema in rats. Results : The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9992) over the linear range. The precisions of intra- and inter-day were less than 7.0% of relative standard deviation (RSD) values for baicalin and less than 3.5% of RDS valuse for glycyrrhizin. Recovery rates were within the range of 95.41-101.5%. The contents of baicalin and glycyrrhizin in SST were average 70.52, 6.18 mg/g, respectively. And SST exhibited inhibitory effect on NO production in LPS-treated RAW 264.7 cells but not on $PGE_2$ production. Oral administration of SST (1 g/kg) showed a reduction in carrageenin-induced paw edema on rats. Conclusions : The analytical method was applied successfully to measure the contents of baicalin and glycyrrhizin in SST which exhibited anti-inflammatory activities.