• Title/Summary/Keyword: 정량한계

Search Result 1,452, Processing Time 0.032 seconds

Analytical Method Development of (-)-Epicatechin gallate in Penthorum chinense Pursh Extract using HPLC (HPLC를 이용한 낙지다리 추출물의 (-)-­Epicatechin gallate 분석법 개발)

  • Kwon, Jin Gwan;Jung, Yeon Woo;Seo, Changon;Hong, Seong Su;Choi, Chun Whan;Lee, Ji Eun;Shin, Hyun Tak;Jung, Su Young;Kim, Jin Kyu
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.45 no.1
    • /
    • pp.87-93
    • /
    • 2019
  • This study attempted to eatablish a High Performance Liquid Chromatography (HPLC) analysis method for the determination of (-)-epicatechin gallate as a part of the quality control for the development of functional cosmetic materials from Penthorum chinense Pursh. HPLC was performed on a Unison $US-C_{18}$ column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and methyl alcohol at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analyte was detected at 280 nm. The HPLC method was performed in accordance with the International Conference on Harmonization (ICH) guideline (version 4, 2005) of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation were 0.11 and 0.33 mg/mL, respectively. Calibration curves showed good linearity ($r^2$ > 0.9999), and the precision of analysis was satisfied (less than 0.6%). Recoveries of quantified compounds ranged from 99.51 to 101.92%. This result indicates that the established HPLC method is very useful for the determination of marker compound in P. chinense Pursh extracts.

Analysis of Cadaverine and Its Worker Honeybee Venom Content (Apis mellifera L.) (꿀벌(Apis mellifera L.) 일벌독의 생체아민 cadaverine 함량 및 분석법)

  • Choi, Hong Min;Kim, Hyo Young;Kim, Se Gun;Han, Sang Mi
    • Journal of Life Science
    • /
    • v.31 no.2
    • /
    • pp.144-148
    • /
    • 2021
  • This study aimed to analyze the content and composition of a biological amine, cadaverine, isolated from the venom of worker honeybees (Apis mellifera L.). This biological amine―which has diverse functionality, such as anti-inflammatory and antibacterial effects―has not been previously reported in bee venom. An assay completed in 13 minutes was developed for the cadaverine present in the bee venom using an ultra-performance liquid chromatograph and a Halo C18 column with acetonitrile and water as the mobile phase. The specificity, accuracy, and precision of the assay were verified, and the assay was validated. The linearity for cadaverine in the bee venom was R2=0.99 or above, indicating a moderate level. The limit of detection and limit of quantification were both 0.3 ㎍/ml, and the rate of recovery was 97.6%-99.1%. The relative standard deviation (RSD) of the intra-day precision and inter-day precision for cadaverine was 0.25%-0.44% and 0.25%-1.25%, respectively, with an RSD that fell within 5% indicating excellent precision. Through this novel assay, it was found that the mean content of cadaverine was 1.10±0.05 mg/g. Our results indicated that the linearity, limit of detection, limit of quantification, and rate of recovery of the cadaverine assay were of a satisfactory level, and the cadaverine content of the bee venom was ably determined. This study provides basic data on cadaverine in bee venom, which will prove useful in further studies on the bioactivity of this component.

Analytical Method Development of Isoscoparin in Silene seoulensis Extract Using HPLC (HPLC 를 이용한 가는장구채 추출물의 Isoscoparin 분석법 개발)

  • Kwon, Jin Gwan;Seo, Changon;Jung, Yeon Woo;Choi, Yongmun;Shin, Hyun Tak;Jung, Su Young;Choi, Jeong June;Kim, Jin Kyu
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.47 no.1
    • /
    • pp.57-63
    • /
    • 2021
  • In this study, isoscoparin was selected as an indicator component to develop Silene seoulensis extract as a functional cosmetic material, and we developed an analysis method using high performance liquid chromatography (HPLC) for quality control. HPLC was performed on a Unison US-C18 with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and methanol at a flow rate of 1.0 mL/min at 35 ℃, and the detection wavelength was 330 nm. The HPLC method was performed in accordance with the international conference on harmonization (ICH) guideline (version 4, 2005) of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation were 0.02 and 0.07 mg/mL respectively. Calibration curves showed good linearity (R2 > 0.99988), and the precision of analysis was satisfied (less than 0.46%). In addition, the recovery rate was in the range of 99.10 to 101.61%, it was shown to be accurate. This result indicated that the established HPLC method is very useful for the determination of marker compounds in Silene seoulensis extracts.

Determination of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) in human urine by solid-phase extraction and GC/MS (고체상 추출과 GC/MS를 이용한 소변 중 대마 대사체 (THCCOOH) 분석)

  • Cheong, Jae Chul;Kim, Jin Young;In, Moon Kyo;Cheong, Won Jo
    • Analytical Science and Technology
    • /
    • v.19 no.5
    • /
    • pp.441-448
    • /
    • 2006
  • 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH) is the major metabolite of tetrahydrocannabinol (THC) which is the primary psychoactive component of marijuana. It is also the target analyte for the discrimination marijuana use. A method using solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of THCCOOH in human urine. Urine samples (3 mL) were extracted by SPE column with a cation exchange cartridge after basic hydrolysis. The eluents were then evaporated, derivatized, and injected into the GC/MS. The limits of detection (LOD) and quantitation (LOQ) were 0.4 and 1.2 ng/mL, respectively. The response was linear with a correlation coefficient of 0.999 within the concentration range of 1.2 (LLE 1.3)~50.0 ng/mL. The precision and accuracy were stable within 1.20% and the recovery was 83.6~90.7%. The recovery of SPE method was lower than that of liquid-liquid extraction (LLE), but there were no apparent differences in LOD, LOQ, precision and accuracy between the two methods. While SPE method is used as a very effective and rapid procedure for sample pretreatment, and clean extracts, LLE method was not suitable for the extraction procedure of THCCOOH in urine. The applicability of the method was proven by analyzing a urine samples from a marijuana abusers.

Validation of enzyme immunoassay for the quantitative measurement of human IgG antibodies specific for Haemophilus influenzae Type b capsular polysaccharide (Haemophilus influenzae type b 피막 다당질 특이 인간 IgG 항체의 정량적 측정을 위한 enzyme immunoassay의 타당성 연구)

  • Kim, Kyung Hyo;Lim, Soo Young
    • Clinical and Experimental Pediatrics
    • /
    • v.50 no.2
    • /
    • pp.143-150
    • /
    • 2007
  • Purpose : This study was conducted to validate enzyme immunoassay (EIA) for the quantitative measurement of human IgG antibodies specific for Haemophilus influenzae type b (Hib) capsular polysaccharide. Method : We evaluated specificity, repeatability, intermediate precision, accuracy, lower limit of quantification (LLOQ), and stability to validate standardized EIA for the quantitative measurement of human anti-polyribosylribitol phosphate (PRP) IgG antibodies. Results : The results indicated that this EIA showed specificity to HbO-HA antigen and repeatability and intermediate precision were within acceptance criteria (repeatability: $CV{\leq}15%$, intermediate precision: $CV{\leq}20%$). The EIA-derived results from this laboratory were equivalent to those obtained by the standard radioactive antigen binding assay (RABA) for quantitation of anti-PRP antibodies in the 28 sera. Spiking recovery result was within acceptance criteria ($100{\pm}20%$). The precision and accuracy of samples in LLOQ were from -14.7 to -4.7% in nominal values, which were within acceptance criteria (precision: $CV{\leq}25%$, accuracy: ${\pm}25%$). Freeze-thaw stability and short term temperature stability were within ${\pm}20%$ of acceptance criteria. Conclusions : The EIA which is performed at the Center for Vaccine Evaluation and Study Ewha Medical Research Institute, is an appropriate serologic assay which can be used for quantitation of anti-PRP IgG antibodies in human sera.

Study for Residue Analysis of Herbicide, Clopyralid in Foods (식품 중 제초제 클로피랄리드(Clopyralid)의 잔류 분석법)

  • Kim, Ji-young;Choi, Yoon Ju;Kim, Jong Su;Kim, Do Hoon;Do, Jung Ah;Jung, Yong Hyun;Lee, Kang Bong;Kim, Hyo Chin
    • Korean Journal of Environmental Agriculture
    • /
    • v.37 no.4
    • /
    • pp.283-290
    • /
    • 2018
  • BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.

A study on the application of the critical strain concept by using the displacements occurring before excavation in tunneling (터널 선행변위를 활용한 한계변형률 개념의 적용 연구)

  • Park, Si-Hyun
    • Journal of Korean Tunnelling and Underground Space Association
    • /
    • v.10 no.4
    • /
    • pp.337-347
    • /
    • 2008
  • Critical strain is a new material property of the ground. Critical strain concept which was established in tunnel engineering can be applied to deformation limits in the ground due to tunneling by using the measured displacement at the tunnel construction site. In this study, quantitative evaluations for the tunnel stability are conducted by analysing the displacement results obtained at the construction field. Especially, critical stain concept was reviewed from a total displacement point of view using the displacements occurring before excavation. As a results, the variation characteristics of the tunnel stability are presented on the critical strain diagram with or without the preceeding displacements.

  • PDF

Determination of Polycyclic Aromatic Hydrocarbons in Processed Chestnut Products (밤가공품 중 polycyclic aromatic hydrocarbons 함량 분석)

  • Seo, Il-Won;Nam, He-Jung;Kim, Dong-Hyuk;Shin, Han-Seung
    • Korean Journal of Food Science and Technology
    • /
    • v.41 no.3
    • /
    • pp.339-344
    • /
    • 2009
  • Concentrations of polycyclic aromatic hydrocarbon (PAH) in processed chestnut products were determined by HPLC/FLD. The methodology involved procedures of sonication with water, extraction with hexane, and clean-up on a Sep-pak florisil cartridge. The PAH limits of detection (LOD) and limits of quantitation (LOQ) ranged from 0.012 to 0.382 ${mu}g/kg$ and from 0.042 to 1.273 ${mu}g/kg$, respectively. The coefficients of variation for intra- and inter-day assays were 0.02-4.48% and 0.37-9.83%, respectively, and the accuracies were 81.95-125.44% and 79.89-116.53%, respectively. The overall recoveries for eight PAHs spiked into the processed chestnut products ranged from 87.83 to 100.56%. As a result, PAH contents were not detected in the processed chestnut products.

A Study on the Neutron Activation Analysis of Noble Metals in the Ancient Coin (고전(古錢)내 귀금속 원소의 중성자 방사화 분석에 관한 연구)

  • Kwon Soo Chun;Chul Lee;Myung-Zoon Czae;Jong Du Lee;Koo Soon Chung
    • Journal of the Korean Chemical Society
    • /
    • v.37 no.11
    • /
    • pp.961-966
    • /
    • 1993
  • The determination of noble metals such as Ir, Au and Ag in the ancient coins has been studied. For the measurement of the activity of $^{192}Ir,\;^{198}Au\;and\;^{110m}Ag$, radiochemical separations including solvent extraction and ion-exchange chromatography were applied to reduce the interference of high energy ${\gamma}$-ray emitted from various radionuclides with long half-life. As a results, $10^{-11}$ g/g level of Ir could be detected and it was found that the three kinds of the detection limits, i.e., critical, detection, quantitative limit, calculated by the method proposed by Currie, were enhanced. Prior to the re-irradiation with neutron, inactive carrier was added in order to determine the recovery yield of Ir in the radiochemical separation. The average recovery yields of Ir, Au and Ag in the 5 coins were 65.3%, 98.5%, 99.5%, respectively.

  • PDF

The analysis of pharmaceuticals in drinking water by HPLC/ESI-MS/MS (HPLC/ESI-MS/MS에 의한 먹는물(정수) 중 의약물질의 분석)

  • Park, Mi-Sun;Kim, Byung-Joo;Myung, Seung-Woon
    • Analytical Science and Technology
    • /
    • v.23 no.5
    • /
    • pp.457-464
    • /
    • 2010
  • The analytical method of four pharmaceuticals (virginiamycin, erythromycin, tylosin and cimetidine) in drinking water was developed. Effective simultaneous sample clean-up and extraction by solid-phase extraction (SPE) using HLB cartridge prior to LC/ESI-MS/MS analysis were performed. A linear correlation observed in the calibration curves for drinking water in the range of 0.01~2.0 ng/mL showed above $r^2$=0.995. Absolute recovery was in the range of 64.7~118.1% (except cimetidine (37.7~48.1%)). Limit of detection (LOD) and limit of quantitation (LOQ) in spiked drinking water matrix were in the range of 1.6~74.8 pg/mL and 5.5~249.7 pg/mL, respectively. The established method can be used to determine low pg/mL levels of pharmaceuticals in the drinking water.