• Title/Summary/Keyword: Phase Calibration

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Determination of eugenol in Eugenia caryophyllata by high-performance Liquid chromatography with photodiode array detection and method validation (HPLC-PDA를 이용한 정향(Eugenia caryophyllata) 중의 eugenol 분석법 확립 및 검증)

  • Yun, Hyeong-Jun;Yun, So-Mi;Lee, Myoung-Heon;Son, Seong-Wan
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.9-16
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    • 2008
  • A method for the quantification of eugenol in the medicinal herb Clove was developed and validated. For preparation of sample solutions clove was dried at $60^{\circ}C$ for 2h and ground by mixer and extracted with 95% ethanol for shaking extraction. The elutes were analyzed by HPLC system included a reversed phase column, a isocratic mobile phase of 60% methanol and PDA detector set at 280 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $0.0125~1{\mu}g/ml$. The limit of detection per sample injection ($20{\mu}l$) was $0.81ng/{\mu}l$ and limit of quantification was $2.47ng/{\mu}l$. The method showed good intra-day precision (%RSD 0.08 ~ 0.27%) and inter-day precision (%RSD 0.32 ~ 1.19%).

Simultaneous Determination of Albiflorin, Cinnamaldehyde, Cinnamic Acid, Daidzin, Glycyrrhizin, Liquiritin, Paeoniflorin and Puerarin in Galgeun-tang by HPLC-PDA

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • The Journal of Korean Medicine
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    • v.31 no.6
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    • pp.8-15
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    • 2010
  • Objectives: We investigated to develop and validate HPLC-PDA methods for simultaneous determination of eight constituents in Galgeun-tang (GGT). Methods: Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 230 nm, 254 nm, and 280 nm, were used for quantification of the eight marker components of GGT. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Results: Calibration curves were acquired with $r^2$ > 0.9999, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 3.0%. The recovery rate of each component was in the range of 87.33-101.38%, with an RSD less than 7.0%. The contents of the eight components in GGT were 1.98-12.17 mg/g. Conclusions: The established method will be applied for the quantification of marker components in GGT.

Method Validation for the Simultaneous Analysis of Organophosphorous Pesticides in Blood by GC/MS (GC/MS를 이용한 혈액 중 유기인제류 농약의 동시 분석에 관한 방법의 유효화)

  • Park Mee Jung;Yang Ja Youl;Kim Ki Wook;Park Yoo Shin;Chung Hee Sun;Lee Sang Ki
    • Environmental Analysis Health and Toxicology
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    • v.20 no.4 s.51
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    • pp.297-302
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    • 2005
  • The purpose of this study was to provide the standard method for the analysis of organophosphorous pesticides such as chlorpyrifos, diazinon, malathion and parathion in blood. We performed method validation for these pesticides in blood according to EURACHEM (A focus For Analytical Chemistry in Europe) guide. For the analysis of the pesticides, we used solid-phase extraction ,column (Waters Oasis $HLB^{(R)}$. After the extraction, the supernatants were evaporated to dryness under the nitrogen stream. They were analyzed by gas chromatography/mass spectrometry (GC/MS) after reconstituting with ethanol. Terbufos was used as an internal standard. To validate this method, we performed verification procedures with the following parameters: selectivity, linearity of calibration, accuracy, precision, limit of detection and quantification. Validation data according to Eurachem guide were adequate for our purpose for the analysis of chlorpyrifos, diazinon, malathion and parathion in blood.

Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs (MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석)

  • 서계원;이재일;이채용;이정치
    • Journal of Food Hygiene and Safety
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    • v.18 no.2
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    • pp.43-50
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    • 2003
  • A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

Simultaneous Determination of Seven Compounds in Samsoeum by HPLC-PDA

  • Seo, Chang-Seob;Kim, Jung-Hoon;Huang, Dae-Sun;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.18 no.1
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    • pp.95-103
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    • 2010
  • Objectives : To develop and validate HPLC-PDA methods for simultaneous determination of seven constituents in Samsoeum(SSE). Methods : Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array(PDA) detection at 254 and 280 nm, were used for quantification of the seven marker components of SSE. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Results : Calibration curves were acquired with $r^2$>0.9997, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 3.0%. The recovery rate of each compound was in the range of 100.07-112.65%, with an RSD less than 4.0%. The contents of seven compounds in SSE were 1.24-10.53 mg/g. Conclusions : The established method will be helpful to improve quality control of SSE.

A Study on Projective Calibration for Arbitrary Display Surface using Digital Moire Method. (Digital Moire를 이용한 임의의 영사면에 대한 투영보정에 관한 연구)

  • 유원재;김도훈;강영준;백성훈
    • Proceedings of the Korean Society of Precision Engineering Conference
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    • 2003.06a
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    • pp.292-295
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    • 2003
  • Moire topography method is a well-known non-contacting 3-D measurement method. the automatic 3-D measurement by moire topography has been required since the method was frequently applied to the engineering and medical fields. 3-D measurement using digital projection moire topography is very attractive because of its high measuring speed and high sensitivity. In this study, digital two-wavelength phase shilling moire is applied to the entertainment fields. recently. as promoting the growth of the VR-Game, display devices which attract public attention such as HMD or Projector are being appeared in order to deliver effectively the absorption sense. this study realized the Auto-calibrating system for arbitrary display surface using digital moire method which satisfied the shape measurement of display surface and the request of FOV(Field of View) output. also when large screen wasn't prepared, this auto-calibrating system was applied to enjoy games or movies at home with a projector and walls

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A Study on the Calibration of Shape Measurement System Using Digital moire (Digital moire 형상측정 시스템의 보정에 관한 연구)

  • 김도훈;유원재;박낙규;강영준
    • Proceedings of the Korean Society of Machine Tool Engineers Conference
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    • 2003.04a
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    • pp.255-259
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    • 2003
  • Moire topography method isa well-known non-contacting 3-D measurement method as afast non-contact test for three-dimension shape measuring method. Recently, it's important to study the automatic three-dimension measurement by moire topography because it is frequently applied to the reverse engineering , the medical , the entertainment fields. Three-dimension measurement using projection of moire topography is very attractive because of its high measuring speed and high sensitivity. In this paper, the classical moire method is computerized-so called digital moire when a virtual grating pattern is projected on a surface, the captured image by the CCD camera has three-dimension information of the objects. The moire image can be obtained through a simple image processing and a reference grating pattern. and it provides similar results without physical grating pattern. digital projection moire topography turn out to be very effective for the three-dimension measurement of objects. Using different N-bucket algorithm method of digital projection moire topography is tested to measuring object with the 2-ambiguity problem. Experimental results prove that the proposed scheme is capable of finding measurement errors that decreased more by using the four-three step algorithm method instead of the same step in the phase shifting of different pitch.

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Sorption Preconcentration and Determination of Nickel in Wastes of Heat Power Industry by Diffuse Reflection Spectroscopy

  • Kalyakina, O.P.;Kononova, O.N.;Kachin, S.V.;Kholmogorov, A.G.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.2
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    • pp.173-177
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    • 2003
  • The present work is focused on the preconcentration of nickel and its determination by means of diffuse reflection spectroscopy. The preconcentration of nickel was carried out by sorption on macroporous aminocarboxylic amphoteric resin ANKB-35. Based on this collector, a method to determine nickel in wastes of heat power industry was worked out using solid-phase spectroscopy. The colored surface compound to be determined was obtained by a preceding nickel sorption on the resin and by subsequent treatment of the concentrate obtained with definite amounts of 1-(2-pyridilazo)-2-naphtol (PAN). The Ni calibration curve is linear in the concentration range of 0.5-20.0 mg/L (sample volume is 200.0 mL) and the detection limit is 0.05 mg/L. The presence of $Cu^{2+},\;Fe^{3+},\;Co^{2+}$ ions as well as macrocomponents of natural water $(Na^+,\;K^+,\;Ca^{2+},\;Mg^{2+})$ do not hinder the solid-phase spectroscopy determination of nickel. The nickel determination by diffuse reflection spectroscopy was carried out in model solutions as well as in solutions obtained after the dissolution of wastes of heat power industry.

UV-HPLC Determination of Carbowyl Group Using 2-Bromoacetyltriphenylene as a Pre-labeling Reagent - The isolative determination of prostaglandin $E_2$ and $F_2{\alpha}$ by HPLC (2-Bromoacetyltriphenylene 유도체화제를 이용한 카르복실기 함유성분의 분석법 (I) - 프로스타글란딘 $E_2$$F_2{\alpha}$ 혼합물의 HPLC에 의한 분리정량)

  • 이왕규;정해수;김박광
    • YAKHAK HOEJI
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    • v.30 no.6
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    • pp.311-316
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    • 1986
  • A new UV labeling reagent was developed and used in HPLC for the determination of prostaglandin $E_2$ which have weak UV light-absorbing property. This reagent, 2-bromoacetyltriphenylene, was synthesized by the bromination of 2-acetyltriphenylene which was obtained from triphenylene by Friedel-Crafts reaction. The wave length maximum (${\lambda}_{max}^{CH_3CN}$ of this reagent was 268nm. Prostaglandin E$_2$ was extracted from prostaglandin E$_2$-$\beta$-cyclodextrin using a Sep-pak $C_{18}$ cartridge. The prostaglandin E$_2$ was labeled with 2-bromoacetyl-triphenylene in aectonitrite using 18-crown-6-ether as catalyst. Derivatized prostaglandins were separated on a reversed-phase column (Radial-pak) $\mu$-Bondapak $C_{18}$ using acetonitrile: water=60:40 as mobile phase. The effluent was monitored by UV detector at 254nm filter kit. Linearity of calibration curve was obtained between 30ng and 140ng, and the lower limit of detection was 5ng.

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Analysis for benzimidazoles in eggs (식용란중 벤지미다졸계 구충제 분석)

  • Kang, Hyung-Joo;Kim, Mun-Bae;Lee, Jae-Bong;Kim, Bong-Sik;Kim, Young-Kab
    • Korean Journal of Veterinary Service
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    • v.26 no.2
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    • pp.157-162
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    • 2003
  • This stud was attempted to detect six benzimidazoles[thiabendazole(TBZ), oxfendazole(OFZ), mebendazole(MBZ), flubendazole(FLBZ), albendazole(ABZ), and febendazole(FBZ)] in eggs using high performance liquid chromatography(HPLC) with photodiode array detector(DAD) simultaneously. The eluates were determined by HPLC on a waters X-Terra$^{TM}\;C_{18}$ reverse-phase column($4.6{\times}250nm,\;5{\mu}m$) with DAD at 295nm. The mobile phase was 0.04M ammonium phosphate(pH 7.5)/ACN(62.28 v/v) run isocratically. The calibration curves were linear(r>0.999) for six benzimidazoles. Average recovery rate from eggs were 94.54% for TBZ, 97.71% for OFZ, 88.82% for MBZ, 93.71% for FLBZ, 78.61% for ABZ, and 75.09% for FBZ, respectively. The limits of detection and quantification were 2.27ppb, 3.88 for TBZ, 9.34ppb, 15.61ppb for OFZ, 28.53ppb, 45.15ppb for MBZ, 27.39ppb, 40.95ppb for FBZ, 8.61ppb, 13.95ppb for ABZ and 12.79ppb, 22.34ppb for FBZ, respectively.