• Title/Summary/Keyword: On-column injection

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Content Analysis of Rutin in the Leaves of Boehmeria nivea Harvested in Different Regions of South Korea by HPLC-UV

  • Cho, Sunghun;Quilantang, Norman G.;Lee, Ju Sung;Kim, Young-Mi;Kim, Ho Bang;Cho, Eun Ju;Jung, Yong-Su;Lee, Sanghyun
    • Natural Product Sciences
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    • v.24 no.1
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    • pp.36-39
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    • 2018
  • Phytochemical analysis of Boehmeria nivea (Bn) leaves by medium pressure liquid chromatography led to the isolation of a flavonoid glycoside identified by spectroscopic analysis as rutin. The amount of rutin in the leaves of Bn harvested from nine regions in South Korea (Bn 1-9) which were collected on the months of June, July, August, and September was determined by HPLC-UV analysis. A gradient elution program that utilizes a $Discovery^{(R)}$ C18 ($4.6{\times}250mm$, $5{\mu}m$) column and mobile phase composed of 1% acetic acid-water: acetonitrile (90:10 to 60:40 for min) was followed. The injection volume and flow rate were $10{\mu}l$ and 1 mL/ min, respectively. UV detection was set at 350 nm. Results show that Bn-8 harvested in September reported the highest content of rutin among the samples analyzed. This study provides a basis for the optimal harvest time of Bn which maximizes the yield of rutin.

Quantitative Determination of Bakkenolide D in Petasites japonicus and Farfugium japonicum by HPLC/UV

  • Quilantang, Norman G.;Lee, Ki Ho;Lee, Dong Gu;Lee, Ju Sung;Cho, EunJu;Kim, Hyun Young;Lee, Sanghyun
    • Natural Product Sciences
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    • v.23 no.4
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    • pp.270-273
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    • 2017
  • A quantitative analysis of bakkenolide D in the different parts of Petasites japonicus and Farfugium japonicum was performed by HPLC. A gradient HPLC elution system with a mobile phase consisting of water: acetonitrile solution (20:80 to 0:100 for 45 min) was followed and an INNO $C_{18}$ column was used for the chromatographic separation. The injection volume, flow rate, and UV detection were $10{\mu}L$, 1 mL/min, and 290 nm, respectively. Results show that both species showed the highest amount of bakkenolide D in the roots being 107.203 and 166.103 mg/g for P. japonicas and F. japonicum, respectively. Content analysis on the different parts of both plants displayed remarkably lower values which ranged from 0.403 - 4.419 and 7.252 - 32.614 mg/g for P. japonicas and F. japonicum, respectively. The results show that the roots of both plants are rich in bakkenolide D showing a promising use in the development of nutraceuticals and industrial application of the compound.

Residual determination of Ceftiofur in Raw Bovine Milk by Liquid Chromatography-Electrospray Mass Spectrometry

  • Lim, Jong-hwan;Park, Byung-kwon;Kim, Myoung-seok;Jang, Beom-Su;Kim, Doo;Yun, Hyo-in
    • Korean Journal of Veterinary Research
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    • v.44 no.3
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    • pp.367-371
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    • 2004
  • This report describes the determination of ceftiofur residues in milk from treatment of lactating dairy cattle by intramuscular injection of three consecutive daily doses of about 1 mg /kg BW, the recommended label dosing. The separation of ceftiofur was achieved on $C_1_8$ reverse phase column. The mobile phase consisted of 0.1% trifluoracetic acid in water (A) and 0.05% acetic acid in acetonitrile (B) and grediently flowed at the flow rate of 0.4 mL/min. As a result of analysis of blank raw bovine milk samples, matrix interference was not shown. Limit of detection and limit of quantitaion was 0.5 ng/mL and 1 ng/mL, respectively. The values of precision and recovery satisfied the guideline of National Veterinary Research and Quarantine Service (NVRQS, Korea). The mean residual concentration of ceftiofur in milk did not exceed 3.71 ng/mL when ceftiofur was administered intramuscularly to lactating dairy cattle for 3 consecutive days at 1 mg/kg of BW per day. It is much lower than the proposed MRL (100 ng/mL) of ceftiofur in milk.

Mornitoring of non-steroidal anti-inflammatory drugs in livestock products (축산식품 중 비스테로이드성 항염증 약물의 잔류함량 모니터링)

  • Choi, Yoon-Hwa;Kim, Yoen-Joo;Shin, Bang-Woo;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.34 no.3
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    • pp.285-289
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    • 2011
  • This study was conducted to determine the content of non-steroidal anti-inflammatory drugs (NSAIDs) in meats available on the Korean markets. The analysis was carried out using following conditions; C18 column ($100{\times}2.1$ mm, 1.7 ${\mu}m$), mobile phase composed of DW (containing 0.1% formic acid): acetonitrile (containing 0.1% formic acid), binary pump at a flow rate of 0.3 ml/min and 5 ${\mu}l$ of injection volume, MS/MS detector with ESI positive mode. The calibration range of five NSAIDs showed linearity ($r^2{\geq}0.99$) at concentration range of 3.125~200 ${\mu}g$/kg. The recoveries in fortified muscle more than 78.7~100.3%. The detection limits for meloxicam, ketoprofen, flunixin, carprofen and tolfenamic acid were 3.5, 1.6, 1.7, 9.8 and 4.8 ${\mu}g$/kg, respectively. We also monitored NSAIDs residue in cattle muscle 51 samples. The test results, NSAIDs were all not founded.

Effect of Bile Salt on the Pharmacokinetics of Bretylium in the Rat (I) - Increased Lipophiiicity of Bretylium by Ion-Pair Complexation with Taurodeoxycholate -

  • Shim, Chang-Koo;Chung, Suk-Jae;Lee, Jeong-Uk;Lee, Min-Hwa;Kim, Shin-Keun
    • Archives of Pharmacal Research
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    • v.9 no.2
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    • pp.111-114
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    • 1986
  • Bretylium tosylate is a quaternary ammonium compound used for the treatment of ventricular fibrilation in humans. It is advantageous to other cationic compound in the study of biliary excretion in that negligible amount is bound to plasma protein and metabolite is not likely is to be formed. Some researchers reported that the formation of ion-pair complex caused to increase the lipothilicity of cationic compound. The partition of bretylium between water and organic phase was increased with the addition of sodium taurodeoxycholate. Also sensitive gas chromatographical assay procedure using flame ionization detector was studied. This procedure can detect as low as 0.1 mg/ml using 0.1 ml biological sample, but contamination by previous injection is the major problem of this method.

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Quantitative Determination of the Six Marker Compounds in Eucommiae Cortex by Processing Method (포제에 따른 두충의 지표성분 함량분석)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo;Kim, Byoung-Soo
    • Korean Journal of Pharmacognosy
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    • v.46 no.2
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    • pp.123-132
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    • 2015
  • In this study, we carried out quantification analysis of the six marker components, geniposidic acid, chlorogenic acid, geniposide, pinoresinol diglucoside, liriodendrin, and genipin in the 70% ethanol extracts of non-processed Eucommiae Cortex and processed Eucommiae Cortex using a high-performance liquid chromatography coupled with photodiode array detector. The six components were separated on Gemini C18 column (5 μm, 4.6×250 mm) by the gradient elution with 1.0% (v/v) acetic acid in water and 1.0% (v/v) acetic acid in acetonitrile as mobile phase. The flow rate was 1.0 mL/min and the injection volume was 10 mL. The amount of geniposidic acid, chlorogenic acid, geniposide, pinoresinol diglucoside, liriodendrin, and genipin in non-processed Eucommiae Cortex were 1.31, 0.31, 0.66, 0.46, 0.46, and 0.03%, respectively, while the amount of the six compounds in non-processed Eucommiae Cortex were 0.04-0.78, 0.01-0.14%, 0.05-0.63%, 0.01-0.37%, 0.15-0.42%, and not detected, respectively. After processing treatment, the contents of three iridoids, two lingnan, and one phenylpropanoid decreased in Eucommiae Cortex.

Quantitative Analysis of the Seventeen Marker Components in Dangguisu-san Using Ultra-performance Liquid Chromatography Coupled to Electrospray Ionization Tandem Mass Spectrometry (LC-MS/MS를 이용한 당귀수산 추출물 중 17종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • YAKHAK HOEJI
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    • v.58 no.3
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    • pp.158-164
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    • 2014
  • Dangguisu-san is a well-known traditional Korean herbal medicine prescription and has been widely used to treat ecchymosis, blood stagnation, and pain resulting from physical shock in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was established for the simultaneous determination of the 17 biomarker components in Dangguisu-san. All analytes were separated on an UPLC BEH $C_{18}$ ($100{\times}2.1$ mm, $1.7{\mu}m$) column and maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in water (A) and acetonitrile (B) by gradient flow. The injection volume was $2.0{\mu}l$ and the flow rate was 0.3 ml/min with detection at mass spectrometer. Calibration curves of the 17 biomarker components were acquired with $r^2$ values ${\geq}0.9951$. The values of limit of detection and quantification of all analytes were 0.02~6.32 ng/ml and 0.05~18.95 ng/ml, respectively. The amounts of the 17 components in Dangguisu-san sample were $3.17{\sim}13,224.50{\mu}g/g$.

Comparison of Extraction Methods for Determination of Vitamin K1 in Vegetables (채소류의 비타민 K1 분석을 위한 추출방법의 비교)

  • Kim, Hyeongi;Choi, Youngmin;Cho, Young-Sook;Sung, Jeehye;Ham, Hyeonmi;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.11
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    • pp.1791-1795
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    • 2014
  • The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.

Characteristics of Dynamic Parameter of Sandy Soil According to Grout Injection Ratio (그라우트 주입율 변화에 따른 사질토의 동적계수 특성)

  • Ahn, Kwangkuk;Park, Junyoung;Oh, Jonggeun;Lee, Jundae;Han, Kihwan
    • Journal of the Korean GEO-environmental Society
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    • v.12 no.5
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    • pp.59-63
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    • 2011
  • Ground dynamic parameter such as shear elastic modulus and damping ratio is a very important variable in design of ground-structure with repeated load and dynamic load. Shear elastic modulus and damping ratio on small strain below linear limit strain is constant regardless of strain. Shear elastic modulus as the maximum shear elastic modulus and damping ratio as the minimum damping ratio were considered. As a lot of experiment related to the maximum shear elastic modulus, which is in dynamic deformation characteristics, have been conducted, many factors including voiding ratio, over consolidation ratio(OCR), confining pressure, geology time, PI, and the number of load cycle affect to dynamic soil characteristic. However, the research of ground dynamic characteristic improved with grout is absent such as underground continuous wall construction, deep mixing method, umbrella arch method. In order to investigate the dynamic soil characteristics improved with grout, in this study, resonant column tests were performed with changing water content(20%, 25%, 30%) and injection ratio of grout(5%, 10%, 15%), cure time(7th day, 28th day) As a result, shear elastic modulus and damping ratio, which are ground dynamic parameter, are affected by the injection ratio of milk grout, cure time and water content.

Study on the Residue Analysis of Organophosphorus and Organochlorine Pesticides with Ion Trap and Quadrupole Mass Spectrometer (Ion Trap Mass Spectrometer와 Quadrupole Mass Spectrometer를 이용한 유기인제 및 유기염소제 농약 분석에 관한 연구)

  • Rhee, Jae-Seong;Park, Hyun-Mee;Er, Yon-Woo
    • Journal of the Korean Chemical Society
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    • v.39 no.12
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    • pp.902-909
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    • 1995
  • Detection limit as well as calibration curves on organophosphorus pesticide(dimethoate, diazinon, parathion-methyl, fenitrothion, malathion) and BHCs were measured for evaluation of utility on qualitative or quantitative analysis of pesticides with ion Trap mass spectrometer and quadrupole mass spectrometer. As ionization source, EI and CI were adopted for qualitative analysis of pesticides by comparison of each fragmentation pattern. At the same time, the utility as trace analysis techniques through scan or selected ion monitoring(SIM) mode was evaluated. With ion trap for all pesticides, detection limit(DL, 1 ${\mu}L$ injection) on scan mode was ranged 0.008∼0.225 ng at signal to noise ratio 3. With quadrupole DL on scan mode was ranged 0.23∼3.1 ng over 0.032∼0.68 ng on SIM mode. The calibration curve with ion trap generated good linearity over 0.99 as correlation coefficient. As clean up procedure, Bio Beads S-X3 was used for the separation of oils from five organophosphorous pesticides in flour extractant showing more than 80% as recovery at most cases. In case of BHCs in jinseng with Florisil column, the recovery of pesticides has been 60% to 90%.

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