• Title/Summary/Keyword: limit of quantification

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Simultaneous Determination of Pesticides in Water Using a GC/MS Coupled with Micro Extraction by Packed Sorbent (MEPS-GC/MS를 이용한 농약류 동시 수질분석)

  • Lee, Ki-chang;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.262-268
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    • 2015
  • This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.

Studies on Analysis Method of T-2 Toxin by ELISA (ELISA에 의한 T-2 toxin의 분석법에 관한 연구)

  • 오유진;장성재;윤여표
    • Journal of Food Hygiene and Safety
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    • v.3 no.2
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    • pp.65-73
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    • 1988
  • T-2 toxin is one of mycotoxins produced by fungi such as Fusarium spp. and possesses a potent cytotoxicity to eukaryotic cell. The contamination of mycotoxins in cereals and feedstuffs is one of the great concerns in health authorities. Therefore, the development of the specific, sensitive and simplified analysis method for T -2 toxin is required. During more than ten years, several chemical and biological analysis methods were proposed and applied for the detection and quantification of T-2 toxin. TLC, GLC-FID and GC-MS are widely employed, but these methods required numerous clean-up procedures before analysis, and the detection limit for T-2 toxin is more than 10 ppb. Biological analysis methods with dermal tissues and cultured cells are not specific to T-2 toxin, since T-2 toxin and other related derivatives possess a similar toxicological activity although their relative activity is different each otber. Based on tbe specific reaction between antibody and antigen, the authors tried to introduce the immunochemical methods for determination of T-2 toxin. The enzyme-linked immunosorbent assay method using monoclonal antibody for T-2 toxin was applied to analyse T-2 toxin. The detection limit of T-2 toxin by ELISA method was 0.1 ppb. The correlation between ELISA and GC-MS method on these samples was very high. ELISA method developed for the detection and quantification of T -2 toxin in this paper possesses simplicity, high sensitivity and specific for T-2 toxin. Furthermore, the ELISA method with T-2 toxin monoclonal antibody was an excellent tool for the screening of Fusarium spp. which was suspected to produce T-2 toxin.

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Plastic Limit Loads for Slanted Circumferential Through-Wall Cracked Pipes Using 3D Finite-Element Limit Analyses (3차원 유한요소 한계해석을 이용한 원주방향 경사관통균열 배관의 소성한계하중)

  • Jang, Hyun-Min;Cho, Doo-Ho;Kim, Young-Jin;Huh, Nam-Su;Shim, Do-Jun;Choi, Young-Hwan;Park, Jung-Soon
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.35 no.10
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    • pp.1329-1335
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    • 2011
  • On the basis of detailed 3D finite-element (FE) limit analyses, the plastic limit load solutions for pipes with slanted circumferential through-wall cracks (TWCs) subjected to axial tension, global bending, and internal pressure are reported. The FE model and analysis procedure employed in the present numerical study were validated by comparing the present FE results with existing solutions for plastic limit loads of pipes with idealized TWCs. For the quantification of the effect of slanted crack on plastic limit load, slant correction factors for calculating the plastic limit loads of pipes with slanted TWCs from pipes with idealized TWCs are newly proposed from extensive 3D FE calculations. These slant-correction factors are presented in tabulated form for practical ranges of geometry and for each set of loading conditions.

Validation of the Analytical Procedure for Quantitative Determination of Four Trace Metals (As, Cd, Pb, and Hg) in Fish Lipids Using Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

  • Kasun S. Jayakody;Ranjith K. B. Edirisinghe;Suchithra A. Senevirathne;Lalith Senarathna
    • Mass Spectrometry Letters
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    • v.15 no.3
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    • pp.149-157
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    • 2024
  • The objective of the present study was to validate the analytical procedure for the quantitative determination of four trace metals (As, Cd, Pb, and Hg) in extracted fish lipids using Inductively Coupled Plasma-Mass Spectrometry, ICP-MS. The extracted lipids using Bligh and Dyer method were digested by means of microwave-assisted acid digestion and introduced into an optimized ICP-MS instrument. The validation of the analytical method was carried out in accordance with the international standards and guidelines outlined in the European Pharmacopeia (2022), which included specificity, selectivity, linearity, limit of detection, limit of quantification, precision, and accuracy. The linearity ranges of the calibration curves were R2 > 0.999, while the relative standard deviation (%RSD) for precision was within 5%. All targeted trace metals have shown mean recoveries between 88.0%-114.9%. The obtained LOD and LOQ values for this analytical protocol indicated the ability to detect and quantify of As, Cd, Pb, and Hg at trace levels. The overall validation confirms the described analytical method was appropriate for routine analyses of As, Cd, Pb, and Hg in fish lipids.

Development and Validation of Quantitative Analysis Method for Phenanthrenes in Peels of the Dioscorea Genus

  • Kim, Hunseong;Cao, Thao Quyen;Yeo, Chae-eun;Shin, Seung Ho;Kim, Hiyoung;Hong, Dong-Hyuck;Hahn, Dongyup
    • Journal of Microbiology and Biotechnology
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    • v.32 no.8
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    • pp.976-981
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    • 2022
  • Phenanthrenes are bioactive phenolic compounds found in genus Dioscorea, in which they are distributed more in peel than in flesh. Recent studies on phenanthrenes from Dioscorea sp. peels have revealed the potential for valuable biomaterials. Herein, an analytical method using high-performance liquid chromatography (HPLC) for quantitation of bioactive phenanthrenes was developed and validated. The calibration curves were obtained using the phenanthrenes (1-3) previously isolated from Dioscorea batatas concentrations in the range of 0.625-20.00 ㎍/ml with a satisfactory coefficient of determination (R2) of 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) values of the isolated phenanthrenes ranged from 0.78-0.89 and 2.38-2.71 ㎍/ml, respectively. The intraday and interday precision ranged from 0.25-7.58%. The recoveries of the isolated phenanthrenes were from 95 to 100% at concentrations of 1.25, 2.5, and 5.0 ㎍/ml. Additionally, phenanthrenes (1-3) were found in all investigated peel extracts. Hence, the developed method was encouraging for the quantitative analysis of phenanthrenes in genus Dioscorea.

Study on the Correlation between the Growth Characteristics and Lignans Contents of Schisandra chinensis (오미자(Schisandra chinensis)의 리그난 함량과 생육특성 간의 상관관계 연구)

  • Dong Hwan Lee;Hyun-Jun Kim;Sun-Young Lee
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2022.09a
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    • pp.101-101
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    • 2022
  • Schisandra chinensis is a fruit which is called Omija in South Korea. The Korean word Omija means "five flavors" (sweet, spicy, sour, bitter, and salty). The aim of his study was to investigate the correlation between growth characteristics and lignans (gomisin A, gomisin N, schisandrin) contents of Schisandra chinensis. The method for determining lignans was validated by measuring the linearity, limit of detection (LOD), limit of quantification (LOQ), precision and accuracy using UPLC-UV. Growth characteristics of S. chinensis such as number of fruits per fruit bunch, length of fruit bunch, width of fruit bunch, fresh weight of fruit bunch, length of fruit, width of fruit, fresh weight of fruit, fresh weight of 30 fruits, and sugar contents of fruit were measured. From the results of correlation analysis, it was found that the contents of lignans showed a significantly negative correlation with fresh weight and sugar contents of fruit. These results will be used to study for quality control of S. chinensis fruit.

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Simultaneous Voltammetric Determination of Mefenamic Acid and Paracetamol using Graphene Nanosheets/Nickel Oxide Nanoparticles Modified Carbon Paste Electrode

  • Naeemy, Ali;Gholam-Shahbazi, Rozhina;Mohammadi, Ali
    • Journal of Electrochemical Science and Technology
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    • v.8 no.4
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    • pp.282-293
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    • 2017
  • A new modified carbon paste electrode (CPE) was constructed based on nickel oxide nanoparticles (NiONPs) and graphene nanosheets (Gr) for simultaneous determination of paracetamol (PCM) and mefenamic acid (MFA) in aqueous media and pharmaceutical dosage forms. NiONPs were synthesized via a simple and inexpensive technique and characterized using X-ray diffraction method. Scanning electron microscopy was used for the characterization of the morphology of modified carbon paste electrode (NiONPs/Gr/CPE). Voltammetric studies suggest that the NiONPs and Gr provide a synergistic augmentation that can increase current responses by improvement of electron transfers of these compounds on the NiONPs/Gr/CPE surface. Using cyclic voltammetry, the NiONPs/Gr/CPE showed good sensitivity and selectivity for the determination of PCM and MFA in individually or mixture standard samples in the linear range of $0.1-30{\mu}g\;mL^{-1}$. The resulted limit of detection and limit of quantification were 20 and $60ng\;mL^{-1}$ for PCM, 24 and $72ng\;mL^{-1}$ for MFA, respectively. The analytical performance of the NiONPs/Gr/CPE was evaluated for the determination of PCM and MFA in pharmaceutical dosage forms with satisfactory results.

Quantitative Analysis of Chrysin and Pinocembrin in Korean Propolis (국산 프로폴리스 내 Chrysin과 Pinocembrin의 정량분석)

  • Kim, Se Gun;Hong, In Pyo;Woo, Soon Ok;Jang, Hye Ri;Han, Sang Mi
    • Korean Journal of Pharmacognosy
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    • v.48 no.1
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    • pp.88-92
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    • 2017
  • In the present study, we carried out quantitative analysis of chrysin and pinocembrin in Korean propolis by ultra performance liquid chromatography (UPLC) equipped with diode array detector. The separation was done using BEH C18 ($2.1{\times}50mm$, $1.7{\mu}m$) column with a mobile phase consisting of MeCN and 0.1% $H_3PO_4$ at 280 nm. The chromatographic method was validated for specificity, limit of detection, limit of quantification, linearity, precision, and accuracy. A quantitative analysis exhibited that the contents of the two compounds in Korean propolis collected from 8 inland areas except Jeju-do ranged from 3.1-46.0 mg/g. These results will be valuable as basic data for standardization of Korean propolis.

A New Analysis of p-Coumaric Acid and Trans-cinnamic Acid in Propolis By UPLC (UPLC를 이용한 프로폴리스 중 p-Coumaric Acid와 Trans-cinnamic Acid 분석법)

  • Kim, Se Gun;Hong, In Pyo;Woo, Soon Ok;Jang, Hye Ri;Han, Sang Mi
    • Korean Journal of Pharmacognosy
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    • v.47 no.2
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    • pp.186-191
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    • 2016
  • A new UPLC-DAD method for simultaneous determination of p-coumaric acid and trans-cinnamic acid in propolis was developed using Halo-C18 column and step gradient elution of MeCN and $0.1%H_3PO_4$ in 8 min. The method was validated by specificity, linearity, limit of detection, limit of quantification, precision(intra- and inter-day variability) and recovery tests. The validated method was sufficiently applicable for quantitative analysis of propolis products as well as propolis collected from different regions in Korea. The established method is simple, appropriate and efficient, and can be used for quality assessment of Korean propolis.

Validation and measurement uncertainty of HPLC method for simultaneous determination of 10 dyes in adulterated Phellodendron

  • Lim, Suji;Yun, Choong-In;Ko, Kyung Yuk;Kim, Young-Jun
    • Korean Journal of Food Science and Technology
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    • v.53 no.4
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    • pp.391-398
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    • 2021
  • As global interest in herbal medicines has increased, the adulteration of herbal medicines has become a critical safety issue. Adulteration with dyes to improve the appearance of low-quality products is of particular concern. This study aimed to develop a high-performance liquid chromatography (HPLC) method to detect dyes added as adulterants to Phellodendron. Samples were analyzed on a C18 column using 50 mM ammonium acetate and acetonitrile as the mobile phase. All calibration curves showed good linearity (r2 ≥0.9999) over the five-point concentration range (1-50 mg/kg). Limit of detection ranged from 0.04-0.35 mg/kg, and limit of quantification ranged from 0.11-1.07 mg/kg. The repeatability and reproducibility for these measurements were 94.2-103.3% and 96.6-103.8% for accuracy and 0.14-2.28 RSD (%) and 0.80-2.37 RSD (%) for precision. Moreover, the measurement uncertainty of the low, medium, and high concentrations for 10 dyes was considered. Thus, this HPLC method is suitable for detecting color adulteration of Phellodendron.