• 제목/요약/키워드: Calibration Curves

검색결과 466건 처리시간 0.024초

Study for Residue Analysis of Fluxametamid in Agricultural Commodities

  • Kim, Ji Young;Choi, Yoon Ju;Kim, Jong Soo;Kim, Do Hoon;Do, Jung Ah;Jung, Yong Hyun;Lee, Kang Bong;Kim, Hyochin
    • 한국환경농학회지
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    • 제38권1호
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    • pp.1-9
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    • 2019
  • BACKGROUND: Accurate and simple analytical method determining Fluxametamid residue was necessary in various food matrices. Additionally, fulfilment of the international guideline of Codex (Codex Alimentarius Commission CAC/GL 40) was required for the analytical method. In this study, we developed Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) method to determine the Fluxametamid residue in foods. METHODS AND RESULTS: Fluxametamid was extracted with acetonitrile, partitioned and concentrated with dichloromethane. To remove the interferences, silica SPE cartridge was used before LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry) analysis with $C_{18}$ column. Five agricultural commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used as a group representative to verify the method. The liner matrix-matched calibration curves were confirmed with coefficient of determination ($r^2$) greater than 0.99 at calibration range of 0.001-0.25 mg/kg. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. Mean average accuracies were shown to be 82.24-115.27%. The precision was also shown to be less than 10% for all five samples. CONCLUSION: The method investigated in this study was suitable to the Codex guideline for the residue analysis. Thus, this method can be useful for determining the residue in various food matrices as routine analysis.

Quantitative analysis method for zingiber officinale water extract using high-performance liquid chromatography

  • Mohd S. Md Sarip;Nik M.A. Nik Daud;Mohd A. Mohd Zainudin;Lokman H. Ibrahim;Syahrul A. Saidi;Zuhaili Idham;Adilah Anuar
    • Advances in materials Research
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    • 제13권3호
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    • pp.233-241
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    • 2024
  • Quantitative analysis of the Zingiber Officinale sample using subcritical water extraction (SWE) was developed employing High-Performance Liquid Chromatography (HPLC) to bolster the advancement of this innovative green extraction process. This research focuses on three principal ginger bioactive compounds: 6-gingerol, 6-shagoal, and 10-gingerol. Various stages were undertaken to establish the quantitative analysis method, encompassing the optimisation of HPLC operating conditions and the formulation of standard calibration curves, yielding individual compound equations. A robust correlation within the calibration curve was achieved, exhibiting an r2 value of 0.9814 and an RSD of 5.00%. A simultaneous, swift, and dependable method was established with an injection time of 20 minutes and an 8-minute delay between injections, in contrast to the previous HPLC analysis requiring a 45-minute injection time for detecting and quantifying all components. Notably, no post-treatment was applied after the SWE process. This advancement allows for potential future online measurement of Zingiber Officinale bioactive compounds extracted using subcritical water extraction through this technology.

전처리 방법에 따른 하수처리장 유입수에서의 미세플라스틱 성상분석 평가 (Evaluation of microplastic in the inflow of municipal wastewater treatment plant according to pretreatment methods)

  • 김성렬;길경익
    • 한국습지학회지
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    • 제24권2호
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    • pp.83-92
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    • 2022
  • 전세계적으로 플라스틱에 대한 수요가 늘어감에 따라 플라스틱 폐기물의 양이 증가하고 있다. 수계 내에서의 미세플라스틱의 위해성에 대한 평가 기준에 대해서는 아직 많은 연구가 필요하지만 대체적으로 미세플라스틱을 성질 개선을 위해 첨가하는 화학물이 유독하다는 사실은 여러 문헌을 통해 증명되어있다. 하수처리장(MWTP)은 오수를 처리하는 시설로서 가정에서 발생하는 미세플라스틱이 모이는 미세플라스틱이 모이는 장소이다. 따라서 MWTP 에서의 미세플라스틱 분석이 필요한 상황이지만 이를 진행하기 위해 표준화된 방법이 아직은 없다. 따라서 본 연구에서는 MWTP에서 미세플라스틱 검출을 위한 하수 시료에 적용할 수 있는 최적의 방법론을 조사해보고자 한다. 본 연구에서는 J 하수 처리장에서 수집한 유입수 샘플로부터 미세플라스틱을 분석하는 다양한 전처리 방법 중에서 하수처리장 샘플에 가장 널리 사용되는 펜톤산화와 H2O2 산화법을 선정하였다. 각 전처리 방법별로 측정에 오차를 발생시킬 요소들이 있었으며, 이를 극복하기 위해 펜톤산화 전처리의 경우 밀도분리법 대신 여과를 진행하여 분석을 진행하는 것이 추천되며, H2O2 산화법의 경우 반응 이후 증류수로 세척하는 과정이 필요해 보인다. 분석 결과 미세플라스틱의 농도는 H2O2 산화법을 이용한 샘플의 경우 2.75 ea/L, 펜톤산화법을 이용한 샘플의 경우 3.2 ea/L 로 측정되었으며 대부분 섬유형태로 존재하였다. 또한 정량분석을 현미경을 이용해 육안으로 진행하기 때문에 측정 결과에 대한 신뢰성을 보장하기가 어렵다고 판단해 검정곡선을 만들었다. 총 3개의 검정곡선이 그려졌으며 해당 검정곡선들을 분석한 결과 R2 값이 전부 0.9 이상이였으며 이는 정량분석에 대해 높은 신뢰성을 보장한다. 정성분석으로 MWTP에 유입되는 미세플라스틱의 계열에 대해선 판단할 수 있었지만 각 미세플라스틱의 화학적인 조성에 대해선 확인할 수 없었다. 향후 MWTP에 유입되는 미세플라스틱의 화학적 조성에 대해서 확인하기 위해서 이번 연구를 활용할 수 있을 것이다.

기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제2보). GLC에 의한 농약의 정량 (Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (II). Determination of Pesticides by GLC)

  • 김택제;박송자;김영상
    • 대한화학회지
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    • 제29권5호
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    • pp.503-509
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    • 1985
  • 농산물에 잔류되어 있는 16종의 유기염소제 농약들을 추출하여 cleanup한 것을 기체 액체 크로마토그래피법으로 분리, 정량하였다. 5% QF-1 정지상의 분리관을 주로 사용하였으며 3% OV-17관과 DC-200/2.5% QF-1 혼합관을 보조적으로 사용하였다. $^{63}Ni$ electron capture detector를 사용하여 각 농약 성분을 검출하였다. 대부분의 농약에 대한 감응곡선은 직선성을 나타냈고 일부는 약간 휘었으나 정량에는 별 지장을 주지 않았다. 16종의 농약을 13종의 농산물에 가하여 분석한 결과 대부분은 85% 이상의 평균회수율을 보였으며 각 5회 분석결과에 대한 상대평균편차는 12.1% 이하로서 AOAC에서 정한 기준을 만족하였다.

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A Breast Cancer Nomogram for Prediction of Non-Sentinel Node Metastasis - Validation of Fourteen Existing Models

  • Koca, Bulent;Kuru, Bekir;Ozen, Necati;Yoruker, Savas;Bek, Yuksel
    • Asian Pacific Journal of Cancer Prevention
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    • 제15권3호
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    • pp.1481-1488
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    • 2014
  • Background: To avoid performing axillary lymph node dissection (ALND) for non-sentinel lymph node (SLN)-negative patients with-SLN positive axilla, nomograms for predicting the status have been developed in many centers. We created a new nomogram predicting non-SLN metastasis in SLN-positive patients with invasive breast cancer and evaluated 14 existing breast cancer models in our patient group. Materials and Methods: Two hundred and thirty seven invasive breast cancer patients with SLN metastases who underwent ALND were included in the study. Based on independent predictive factors for non-SLN metastasis identified by logistic regression analysis, we developed a new nomogram. Receiver operating characteristics (ROC) curves for the models were created and the areas under the curves (AUC) were computed. Results: In a multivariate analysis, tumor size, presence of lymphovascular invasion, extranodal extension of SLN, large size of metastatic SLN, the number of negative SLNs, and multifocality were found to be independent predictive factors for non-SLN metastasis. The AUC was found to be 0.87, and calibration was good for the present Ondokuz Mayis nomogram. Among the 14 validated models, the MSKCC, Stanford, Turkish, MD Anderson, MOU (Masaryk), Ljubljana, and DEU models yielded excellent AUC values of > 0.80. Conclusions: We present a new model to predict the likelihood of non-SLN metastasis. Each clinic should determine and use the most suitable nomogram or should create their own nomograms for the prediction of non- SLN metastasis.

Discrete element numerical simulation of dynamic strength characteristics of expanded polystyrene particles in lightweight soil

  • Wei Zhou;Tian-shun Hou;Yan Yang;Yu-xin Niu;Ya-sheng Luo;Cheng Yang
    • Geomechanics and Engineering
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    • 제34권5호
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    • pp.577-595
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    • 2023
  • A dynamic triaxial discrete element numerical model of lightweight soil was established using the discrete element method to study the microscopic mechanism of expanded polystyrene (EPS) particles in the soil under cyclic loading. The microscopic parameters of the discrete element model of the lightweight soil were calibrated depending on the dynamic triaxial test hysteresis curves. Based on the calibration results, the effects of the EPS particles volume ratio and amplitude on the contact force, displacement field, and velocity field of the lightweight soil under different accumulated strains were studied. The results showed that the hysteresis curves of lightweight soil exhibit nonlinearity, hysteresis, and strain accumulation. The strain accumulated in remolded soil is mainly tensile strain, and that in lightweight soil is mainly compressive strain. As the volume ratio of EPS particles increased, the contact force first increased and then decreased, and the displacement and velocity of the particles increased accordingly. With an increase in amplitude, the dynamic stress of the particle system increased, and the accumulation rate of the dynamic strain of the samples also increased. At 5% compressive strain, the contact force of the particles changed significantly and the number of particles deflected in the direction of velocity also increased considerably. These results indicated that the cemented structure of the lightweight soil began to fail at a compressive strain of 5%. Thus, a compressive strain of 5% is more reasonable than the dynamic strength failure standard of lightweight soil.

유리섬유 부직포가 삽입된 풍력 블레이드 인발 성형 스파캡 소재의 파괴인성 특성 평가 (Evaluation of Fracture Toughness Characteristics of Pultruded CFRP Spar-Cap Materials with Non-woven Glass Fabric for Wind Blade)

  • 김영철;주근수;박지상;이우경;강민규;김지훈
    • 풍력에너지저널
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    • 제14권3호
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    • pp.83-90
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    • 2023
  • The purpose of this study is to evaluate the inter-laminar fracture toughness characteristics of CFRP pultrusion spar cap materials reinforced with non-woven glass fabric. Test specimens were fabricated by the infusion technique. A non-woven glass fabric and artificial defects were embedded on the middle surface between two pultruded CFRP panels. Double cantilever beam (DCB) and End Notched Flexure (ENF) tests were performed according to ASTM standards. Fracture toughness and crack propagation characteristics were evaluated with load-displacement curves and delamination resistance curves (R-Curve). The fracture toughness results were calculated by compliance calibration (CC) method. The initiation and propagation values of Mode-I critical strain energy release rate value GIc were 1.357 kJ/m2 and 1.397 kJ/m2, respectively, and Mode-II critical strain energy release rate values GIIc were 4.053 kJ/m2 for non-precracked test and 4.547 kJ/m2 for precracked test. It was found that the fracture toughness properties of the CFRP pultrusion spar-cap are influenced by the interface between the layers of CFRP and glass fiber non-woven.

Analysis of Cationic Surfactants in Cosmetics By Reverse phase Ion-Pair Chromatigraphy with Suressed Conductivity Detector and UV Detector

  • Jong-Keun Choi;Jae
    • 대한화장품학회지
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    • 제23권3호
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    • pp.161-167
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    • 1997
  • Determination of several cationic surfactants in cosmetics has been investigated. Reverse phase ion pair chromatography was used to identify and quantitate cationic surfactants. Cationic surfactants analyzed in this experiment were cetylpyridium chloride, stearyltrimetylammonium chloride, bezalkonium chloride, benzyldicethylcetylammonium chloride, and bihenyltrimethyl ammonium chloride. The separation was achieved on a reverse phase coumn with 10mM HCl-acetonitrile eluent. In this condition, the most of cationic surfactants with exception of CPC and CTAC respectively with suppressed conductivity detector and UV detector connected in series. The calibration curves obtained by plotting the peak areas of the cationic surfactants were linear at levels ranging from 0.005 to 0.1% correlation coefficient, r=0.9988. The detection limits were 1 to 5ppm in sample solution. The average recoveries of cationic surfactants added to hair treatment cream and hair rinse in three to five experiments were 96.7 105.2% and relative standard deviations were 1.1-3.8%. The case that there were CPC and CTAC in same solution was also tested. CPC and CTAC which couldn't be separated on reverse phase column were quantitated with suppressed conductivity detector and UV detector connected in series. Recovery of CPC and CTAC were 101.6 and 89.2% respectively. The proposed method was applied to the determination of cationic surfactants in commercial hair treatment cream.

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Determination of Coccidiostats (Amprolium and Decoquinate) in Cattle and Chicken's Muscle using High Performance Liquid Chromatography

  • Kim, Byung-Ju;Ham, Hyun-Sun;Lee, Jin-Joo;Cheong, Nam-Yong;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • 제33권2호
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    • pp.559-563
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    • 2012
  • An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

역상 액체크로마토그래피에 의한 1-(2-Pyridylazo)-2-Naphthol과 킬레이트를 형성하는 금속이온의 분리 (Reversed-Phase Liquid Chromatographic Separation of Metal Ions by Chelate Formation with 1-(2-Pyridylazo)-2-Naphthol)

  • 강삼우;박선자
    • 대한화학회지
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    • 제42권2호
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    • pp.197-202
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    • 1998
  • 1-(2-Pyridylazo)-2-Naphthol (PAN)은 많은 금속이온들과 착색된 착물을 형성함으로 분광시약 또는 금속지시약으로 널리 사용된다. 본 연구는 PAN을 이동상에 첨가하여 Cu(II), Ni(II) , Zn(II), Co(II) , 및 Fe(III)이온들과 착물을 형성시켜 역상 액체크로마토그래피법으로 분리하였다. 이들 금속착물들은 570nm에서 분광광도 검출기로 검출되었고, 이들 금속이온의 머무름을 조사하기 위하여 이동상의 pH, 이온세기 및 유기용매 조성의 변화에 따른 크로마토그램과 용량인자를 측정하였다. 이상의 실험결과에서 얻은 최적조건하에서 금속이온을 분리한 결과 좋은 크로마토그램을 얻었으며, 검출한계(S/N)도 ppb단위까지 검출이 가능함을 알 수 있었다.

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