• Title/Summary/Keyword: 정량검출한계

Search Result 668, Processing Time 0.025 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.

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.

Survey and method validation of simultaneous quantitative analysis of T-2 and HT-2 toxins in cereals (곡류 중 T-2 및 HT-2 독소 동시 정량분석의 유효성 검증 및 실태조사)

  • Paek, Ockjin;Kang, Teabeom
    • Food Science and Preservation
    • /
    • v.22 no.4
    • /
    • pp.559-566
    • /
    • 2015
  • The aim of this study was to develop an analytical method for determination of T-2 toxin and HT-2 toxin level in cereals and to survey their levels using LC-MS/MS. The T-2 and HT-2 toxins were simultaneously analyzed by electrospray ionization with a positive ion mode and multiple reaction monitoring (MRM) after filteration and immuno-affinity column clean-up. A matrix-matched standard calibration used for quantification and recoveries of T-2 and HT-3 toxins were in the range of $100.6{\pm}7.2%$ and $96.8{\pm}9.4%$, respectively. Limits of detection and quantification of T-2 and HT-2 toxins were estimated to be 0.5 and $1.5{\mu}g/kg$, respectively. Each repeatability (RSRr) of T-2 and HT-2 toxins was determined to be 0.9~6.0%, and 4.9~6.1%, respectively. Total 115 samples cereals were collected from 9 types of cereals for analysis. The positive percentages of T-2 and HT-2 toxins obtained from collected samples were found to be 72% and 80%, respectively. The contamination level of T-2 toxin and HT-2 toxin in cereals were $37.1{\mu}g/kg$, and $5.4{\mu}g/kg$, respectively. Therefore, this study suggests that the developed method could be an useful analytical method to determine the T-2 and HT-2 toxin level in cereals and the present data could be used as a reference to estimate the risk assessment.

Improvement of the detection limit of rapid detection kit for Salmonella Typhimurium using image analysis system (이미지 분석을 이용한 살모넬라 신속 진단키트의 측정감도 향상)

  • Lee, Sangdae;Kim, Giyoung;Park, Saet-Byeol;Moon, Ji-Hea
    • Korean Journal of Agricultural Science
    • /
    • v.39 no.3
    • /
    • pp.421-425
    • /
    • 2012
  • The objective of this study was to improve the detection limit of rapid detection kit for Salmonella Typhimurium by image analysis system. The rapid detection kit was comprised of four elements: sample pad, conjugate pad, nitrocellulose pad and absorbent pad. Gold nanoparticle and Salmonella antibody were used as a tag and a receptor. Salmonella antibody and goat rabbit IgG antibody were used as test and control lines on nitrocellulose membrane. The color intensity of test line began to increase from $10^5CFU/mL$ of Salmonella sample. A multiple linear regression analysis was employed to explain the relationship between predicted and measured number of Salmonella cells. The developed model could successfully predict the cell number of Salmonella with validation against extra-experimental result.

Photometric Determination of Chlorite ion by Flow Injection Analysis (흐름주입 분석에 의한 아염소산 이온의 분광광도법 정량)

  • Choi, Yong Wook;Lee, Su Young;Kim, Mi Kyung;Park, Sung Ho
    • Journal of the Korean Chemical Society
    • /
    • v.44 no.6
    • /
    • pp.556-562
    • /
    • 2000
  • The determination of chlorite ion by flow injection analysis(FIA) with iodometric UV detection were investigated. Under rather acidic condition, chlorite ion react with iodide ion to form iodine and itself is reduced to chloride ion. The chlorite ion was determined indirectly by measuring absorbance of yellow colored iodine at 370 nm. The lengths of the mixing coil and the reaction coil, the pH of the acid stream, the concentration of the iodide ion, the injection loop volume, temperature, and flowrate were optimized as parameters for selectively determining a sort of inorganic disinfection by-product, chlorite ion by using FIA-UV detection setup. Masking agents for removing oxidants or interferences from the prepared water were tested. Independent calibration curve presented linear range of 0.002-0.2 mg/L for chlorite ion with a correlation coefficient of 0.999 or better. The limit of detection(LOD) was 0.18 ${\mu}g/L$ for chlorite ion.

  • PDF

Spectrophotometric Quantitatification of Fe(II) and Fe(III) Ions Using N,N'-bis(4-methoxysalicylidene) phenylendiamine (N,N'-bis(4-methoxysalicylidene) phenylendiamine를 이용한 Fe(II) 및 Fe(III) 이온의 분광학적 분석)

  • Kim, Sun-Deuk;Seol, Jong-Min
    • Journal of the Korean Chemical Society
    • /
    • v.55 no.3
    • /
    • pp.463-471
    • /
    • 2011
  • A novel $N_2O_2$ Schiff base ligand, N,N'-bis(4-methoxysalicylidene)phenylendiamine(4-$CH_3O$-Salphen), has been synthesized. It has been revealed that the compound is very useful for the spectrophotometric quantification of Fe(II) and Fe(III) ions in aqueous solutions, such as mineral water, hot spring water, sea water, and waste water. The optimum conditions for the quantitative analysis are the followings; [4-$CH_3O$-Salphen]=$4.0{\times}10^{-4}\;M$, DMF/$H_2O$=70/30(v/v), pH=3.4~3.8, T= at $55^{\circ}C$, and prereaction time=1.0 hr. The sample of single valence state was prepared by the preliminary oxidation or reduction using $H_2O_2$ ($5.0{\times}10^{-4}\;M$) and $NH_2OH{\cdot}HCl$ ($5.0{\times}10^{-4}\;M$). The quantitative analyses of Fe(II) and Fe(III) ion were performed by measuring the absorbance at 434 nm and 456 nm, respectively. The estimated mean values agreed well with the standard values within the range of 2.00~6.90%. The limit of detection was 27.9 ng/mL for Fe(II) and 55.8 ng/mL for Fe(III).

Determination of Rh(III) by Spectrofluorimetry Using Oxidation Reaction of Nile Blue (Nile Blue의 산화반응을 이용한 Rh(III)의 형광분광법적 정량)

  • Lee, Sang Hak;Lee, Myeong
    • Journal of the Korean Chemical Society
    • /
    • v.45 no.1
    • /
    • pp.25-30
    • /
    • 2001
  • A selective kinetic fluorimetric method for the determination of trace rhodium(Ⅲ), based on the catalytic effect of rhodium(Ⅲ) on the oxidation of nile blue by periodate have been studied. The effects of pH and concentrations of nile blue, sodium periodate, trioctyl phosphine oxide(TOPO) and temperature were investigated. The calibration curve for rhodium(Ⅲ) ion was linear over the range from 100 ng/mL to 0.1 ng/mL and the detection limit was 0.01 ng/mL under the optimal experimental conditions. Effects of interferences from several cations and anions for the determination of rhodium(Ⅲ) were also investigated.

  • PDF

Determination of N-nitrosamines in Water by Gas Chromatography Coupled with Electron Impact Ionization Tandem Mass Spectrometry (EI-GC/MS/MS를 이용한 니트로사민류의 수질분석)

  • Lee, Ki-Chang;Park, Jae-Hyung;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.36 no.11
    • /
    • pp.764-770
    • /
    • 2014
  • This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

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.

Determination of Preservatives in Raw Materials of Functional Foods by HPLC-PDA and GC-FID (HPLC 및 GC를 이용한 건강기능식품 원료 중 보존료 함유량 조사)

  • Kim, Jung-Bok;Kim, Myung-Chul;Song, Sung-Woan;Shin, Jae-Wook
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.46 no.3
    • /
    • pp.358-367
    • /
    • 2017
  • Preservatives, as food additives, are occasionally intrinsic to natural raw materials or sometimes generated during the fermentation process as reported in many research articles. Preservative compounds in raw food materials may persist in the final food product, which is not supposed to include such preservative compounds. In this study, we validated an analytical method for preservative compounds in raw materials of functional foods. Quantification of benzoic acid and sorbic acid was determined using HPLC-PDA analysis after distillation, whereas propionic acid was quantified with GC-FID. A significant set of validation data (accuracy, precision, linearity, recovery, etc) was acquired. A total of 212 samples were collected for analysis of naturally occurred preservatives, and preservatives were detected in 85 samples. Most of the detected samples showed less 10 mg/kg of preservatives. The results of this study provide fundamental data on naturally occurring preservatives in raw materials of functional foods. Moreover, building up a database of naturally occurring preservatives could solve problems in the current scientific data.