• 제목/요약/키워드: standard calibration

검색결과 1,151건 처리시간 0.028초

LC-MS/MS를 이용한 축·수산물 중 β-agonist계 시험법 개발 및 검증 (Development and Validation of an Analytical Method for β-Agonists in Livestock and Fishery Products Using LC-MS/MS)

  • 이태호;김유라;박수정;김지영;최장덕;문귀임
    • 한국환경농학회지
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    • 제41권2호
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    • pp.135-151
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    • 2022
  • BACKGROUND: The β-agonists known as phenyl ethanolamine derivatives have a conjugated aromatic ring with amino group. They are used as tocolytic agents and bronchodilator to human and animal generally, and some of them are used as growth promoters to livestock. METHODS AND RESULTS: β-agonists in samples were extracted by 0.4 N perchloric acid and ethyl acetate. The target compounds were analyzed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS). Validation of method was performed according to CODEX guidelines (CAC/GL-71). The matrix matched calibration gave correlation coefficients>0.98, and the obtained recoveries were in the range of 62.0-109.8%, with relative standard deviation ≤ 20.1%. In addition, a survey was performed to inspect any residual β-agonist from 100 samples of livestock and fishery products and ractopamine was detected in one of the 100 samples. CONCLUSION(S): In this study, we established the analytical method for β-agonists through using the expanded target compounds and samples. And we anticipate that the established method would be used for analysis to determine veterinary drug residues in livestock and fishery products.

CHEMICAL AND MICROBIOLOGICAL ANALYSIS OF GOAT MILK, CHEESE AND WHEY BY NIRS

  • Perez Marin, M.D.;Garrido Varo, A.;Serradilla, J.M.;Nunez, N.;Ares, J.L.;Sanchez, J.
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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    • pp.1513-1513
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    • 2001
  • Present Food Legislation compels dairy industry to carry out analyses in order to guarantee the food safety and quality of products. Furthermore, in many cases industry pays milk according to bacteriological or/and nutritional quality. In order to do these analyses, several expensive instruments are needed (Milkoscan, Fossomatic, Bactoscan). NIRS technology Provides a unique instrument to deal with all analytical requirements. It offers as main advantages its speed and, specially, its versatility, since not only allows determine all the parameters required in milk analysis, but also allows analyse other dairy products, like cheese or whey. The objective of this study is to develop NIRS calibration equations to predict several quality parameters in goat milk, cheese and whey. Three sets of 123 milk samples, 190 cheese samples and 109 whey samples, have been analysed in a FOSS NIR Systems 6500 I spectrophotometer equipped with a spinning module. Milk and whey were analysed by folded transmission, using circular cells with gold surface and pathlength of 0.1 m, while intact cheese was analysed by reflectance using standard circular cells. NIRS calibrations were obtained for the prediction of chemical composition in goat milk, for fat (r$^2$=0.92; SECV=0.20%), total solids (r$^2$=0.95: SECV=0.22%), protein (r$^2$=0.94; SECV=0.07%), casein (r$^2$=0.93; SECV=0.07%) and lactose (r$^2$=0.89; SECV=0.05%). Moreover, equations have been performed to determine somatic cells (r$^2$=0.81; SECV=276.89%) and total bacteria (r$^2$=0.58; SECV=499.32%) counts in goat milk. In the case of cheese, calibrations were obtained for the prediction of fat (r$^2$=0.92; SECV=0.57), total solids (r$^2$=0.80; SECV=0.92%) and protein (r$^2$=0.70; SECV=0.63%). In whey, fat (r$^2$=0.66; SECV=0.08%), total solids (r$^2$=0.67; SECV=0.19%) and protein (r$^2$=0.76; SECV=0.07%) NIRS equations were obtained. These results proved the viability of NIRS technology to predict chemical and microbiological parameters and somatic cells count in goat milk, as well as chemical composition of goat cheese and whey.

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THE USE OF NEAR INFRARED REFLECTANCE SPECTROSCOPY(NIRS) TO PREDICT CHEMICAL COMPOSITION ON MAIZE SILAGE

  • D.Cozzolino;Fassio, A.;Mieres, J.;Y.Acosta
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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    • pp.1610-1610
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    • 2001
  • Microbiological examination of silage is of little value in gauging the outcome of silage, and so chemical analysis is more reliable and meaningful indicator of quality. On the other hand chemical assessments of the principal fermentation products provide an unequivocal basis on which to judge quality. Livestock require energy, protein, minerals and vitamins from their food. While fresh forages provide these essential items, conserved forages on the other hand may be deficient in one or more of them. The aim of the conservation process is to preserve as many of the original nutrients as possible, particularly energy and protein components (Woolford, 1984). Silage fermentation is important to preservation of forage with respect of feeding value and animal performance. Chemical and bacteriological changes in the silo during the fermentation process can affect adversely nutrient yield and quality (Moe and Carr, 1984). Many of the important chemical components of silage must be assayed in fresh or by extraction of the fresh material, since drying either by heat or lyophilisation, volatilises components such as acids or nitrogenous components, or effects conversion to other compounds (Abrams et al., 1987). Maize silage dorms the basis of winter rations for the vast majority of dairy and beef cattle production in Uruguay. Since nutrient intake, particularly energy, from forages is influenced by both voluntary dry matter intake and digestibility; there is a need for a rapid technique for predicting these parameters in farm advisory systems. Near Infrared Reflectance Spectroscopy (NIRS) is increasingly used as a rapid, accurate method of evaluating chemical constituents in cereals and dried forages. For many years NIRS was applied to assess chemical composition in dry materials (Norris et al., 1976, Flinn et al., 1992; Murray, 1993, De Boever et al., 1996, De la Roza et al., 1998). The objectives of this study were (1) to determine the potential of NIRS to assess the chemical composition of dried maize samples and (2) to attempt calibrations on undried samples either for farm advisory systems or for animal nutrition research purposes in Uruguay. NIRS were used to assess the chemical composition of whole - plant maize silage samples (Zea mays, L). A representative population of samples (n = 350) covering a wide distribution in chemical characteristics were used. Samples were scanned at 2 nm intervals over the wavelength range 400-2500 nm in a NIRS 6500 (NIRSystems, Silver Spring, MD, USA) in reflectance mode. Cross validation was used to avoid overfitting of the equations. The optimum calibrations were selected on the basis of minimizing the standard error of cross validation (SECV). The calibration statistics were R$^2$ 0. 86 (SECV: 11.4), 0.90 (SECV: 5.7), 0.90 (SECV: 16.9) for dry matter (DM), crude protein (CP), acid detergent fiber (ADF) in g kg$\^$-1/ on dry matter, respectively for maize silage samples. This work demonstrates the potential of NIRS to analyse whole - maize silage in a wide range of chemical characteristics for both advisory farm and nutritive evaluation.

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LC-MS/MS를 이용한 농산물 중 제초제 Sulfonylurea계 36종 동시 시험법 개발 (Development of the Simultaneous Analysis of 36 Sulfonylurea Herbicide Residues in Agricultural Products Using LC-MS/MS)

  • 이수정;이정미;장귀현;김현경;김지영
    • 한국환경농학회지
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    • 제42권2호
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    • pp.139-151
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    • 2023
  • Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO4 and C18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R2) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

가스크로마토그래프-질량분석기에 의한 타액 및 뇨 중 포름알데하이드 분석법 연구 (The study on the measurement of formaldehyde in saliva and urine by GC-MS)

  • 신호상;안혜실
    • 분석과학
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    • 제19권2호
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    • pp.149-154
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    • 2006
  • 가스크로마토그래프-질량분석기를 사용한 타액과 뇨 시료 중 포름알데하이드의 분석법이 확립되었다. 타액 또는 뇨 시료 0.2 ml를 20 mL 유리시험관에 넣고 0.1 M HCl 1.8 ml와 내부표준물질인 20 mg/L acetone-$d_6$$20{\mu}l$ 그리고 2,000 mg/L 2,4-dinitrophenyl hydrazine을 0.1 mL첨가하여 진탕기로 실온에서 20분간 반응시켰다. 반응 후 toluene 4 mL를 넣어 추출하여 원심분리 후 toluene 층을 분리하고 완전 농축시킨 후 acetonitrile $100{\mu}l$로 재 용해시켜 가스크로마토그래프-질량분석기로 측정하였다. 이때 검출한계는 타액 중에서는 2.0 ng/mL 이었고 뇨 중에서는 0.5 ng/mL이었다. 검량선은 타액과 뇨 중에서 각각 0.997과 0.998로 좋은 직선성을 보였다. 이 방법은 포름알데하이드를 구강 노출시킨 쥐의 뇨 중에서 포름알데하이드를 검출하는데 사용하였으며 사람의 뇨나 타액에서 포름알데하이드를 검출하는 데에도 가치 있는 방법으로 사료된다.

HPLC-MS/MS에 의한 감초의 liquiritin과 glycyrrhizin의 분석 (Qunatitative analysis of liquiritin and glycyrrhizin in glycyrrhizae radix by HPLC-MS/MS)

  • 유영법;김미정;황대선;하혜경;마진열;신현규
    • 분석과학
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    • 제20권4호
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    • pp.331-338
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    • 2007
  • 한약과 기능성식품으로 널리 활용되는 감초의 지표물질인 glycyrrhizin과 liquiritin을 HPLC-MS/MS 로 정성, 정량분석을 실시하였다. 두 가지 지표성분 모두 positive ion mode에서 검출이 가능하였고, precursor ion과 product ion을 조합한 multiple-reaction monitoring (MRM) mode에서 liquiritin은 m/z $436.2{\rightarrow}257.0$로 관찰되었고, glycyrrhizin은 m/z $823.4{\rightarrow}453.4$ 로 각각 검지되었다. 감초 물 추출물을 분무건조기로 건조한 분말에서 glycyrrhizin의 경우 5.8%, liquiritin의 경우 2.3% 각각 함유되어 있었다. 회수율은 103-113%였고, 일간, 일내 정밀도 실험에서 상대표준편차는 0.95-1.8% 였다. 본 실험 조건에서 liquiritin과 glycyrrhizin의 검출한계는 각각 0.4 ng/mL과 0.01 ng/mL 이었다.

다차원 공간정보 기반의 충주댐 저수용량 비교분석 (The Comparative Analysis of Reservoir Capacity of Chungju Dam based on Multi Dimensional Spatial Information)

  • 이근상
    • 대한토목학회논문집
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    • 제30권5D호
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    • pp.533-540
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    • 2010
  • 댐은 용수공급 및 홍수조절을 위한 매우 중요한 시설물이며, 따라서 댐의 효율적인 관리를 위해서는 저수용량을 정확히 분석하는 연구가 필요하다. 본 연구에서는 충주댐 저수지를 대상으로 다차원공간정보를 이용하여 시계열 저수용량 비교하였으며 주요 결론은 다음과 같다. 먼저 댐 저수지 주변의 육상부와 수심부에 각각 LiDAR와 MBES 측량을 수행하였으며, 측량자료의 정확도 향상을 위해 캘리브레이션 보정과정을 실시한 후 지상기준점과의 검정을 통해 허용오차 기준을 만족하는 다차원공간정보를 구축할 수 있었다. 항공 LiDAR와 MBES 자료를 연계하여 생성한 정밀지형자료로부터 불규칙삼각망 모델을 이용하여 수위별 저수용량을 계산하였으며 회귀분석을 통해 2008년도 저수용량 곡선식을 개발하였다. 2008년도 저수용량을 1986년과 1996년과 비교한 결과, 저수지 퇴사증가로 인해 수위가 높아질수록 총저수용량은 감소하는 추세를 보였다. 또한 수위 구간별로 저수용량을 계산하여 침식과 퇴사가 나타나는 구간을 분석할 수 있었으며, 특히 1986~2008년과 1996~2008년 동안의 평균수위 직상부 구간인 130.0~135.0m에서 가장 많은 침식특성이 나타났으며 이는 집중강우로 인해 저수지 사면침식이 주요 원인으로 판단된다.

액체크로마토그래피를 이용한 화장품 제형 내 세라마이드엔피 분석법 확립 (Development of Ceramide NP Analysis Method in Cosmetic Formulations Using Liquid Chromatography)

  • 이예지;김영은;서재용;조현대
    • 대한화장품학회지
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    • 제49권4호
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    • pp.291-298
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    • 2023
  • 본 연구에서는, 화장품 중 로션, 크림, 클렌저 제형에 적용된 세라마이드엔피(ceramide NP)의 함량을 분석하고자 high-performance liquid chromatography (HPLC)를 이용한 정량 분석 방법을 개발하였다. 분석은 C18 칼럼을 이용하고 이동상은 아세토니트릴과 메탄올을 70 : 30 비율로, 유속은 0.8 mL/min으로 하고 칼럼 온도는 20 ℃로 조건을 설정하였다. 분석 방법은 ICH 가이드라인에 따라 특이성, 직선성, 검출한계(LOD) 및 정량한계(LOQ), 정확성, 정밀성을 분석하여 검증하였다. 분석 방법의 유효성 검증 결과, 검량선의 직선성(R2)은 0.99984로 우수한 직선성을 보였다. 로션, 크림, 클렌저 제형에 대한 정확성은 95.11 ~ 100.48%의 회수율을 통해 확인하였고, 정밀성 분석 결과 상대 표준 편차(RSD)는 0.26% 이하로 나타났다. 검출한계는 0.902 ㎍/mL, 정량한계는 2.733 ㎍/mL로 확인되었다. 이를 통해, 화장품에 적용된 세라마이드엔피의 정량 분석 시, 방해 물질의 영향으로 인해 주피크 분리가 어려운 경우 측정이 가능하게 하여 제품의 품질관리에 도움이 될 것으로 기대된다.

Feasibility of a Clinical-Radiomics Model to Predict the Outcomes of Acute Ischemic Stroke

  • Yiran Zhou;Di Wu;Su Yan;Yan Xie;Shun Zhang;Wenzhi Lv;Yuanyuan Qin;Yufei Liu;Chengxia Liu;Jun Lu;Jia Li;Hongquan Zhu;Weiyin Vivian Liu;Huan Liu;Guiling Zhang;Wenzhen Zhu
    • Korean Journal of Radiology
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    • 제23권8호
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    • pp.811-820
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    • 2022
  • Objective: To develop a model incorporating radiomic features and clinical factors to accurately predict acute ischemic stroke (AIS) outcomes. Materials and Methods: Data from 522 AIS patients (382 male [73.2%]; mean age ± standard deviation, 58.9 ± 11.5 years) were randomly divided into the training (n = 311) and validation cohorts (n = 211). According to the modified Rankin Scale (mRS) at 6 months after hospital discharge, prognosis was dichotomized into good (mRS ≤ 2) and poor (mRS > 2); 1310 radiomics features were extracted from diffusion-weighted imaging and apparent diffusion coefficient maps. The minimum redundancy maximum relevance algorithm and the least absolute shrinkage and selection operator logistic regression method were implemented to select the features and establish a radiomics model. Univariable and multivariable logistic regression analyses were performed to identify the clinical factors and construct a clinical model. Ultimately, a multivariable logistic regression analysis incorporating independent clinical factors and radiomics score was implemented to establish the final combined prediction model using a backward step-down selection procedure, and a clinical-radiomics nomogram was developed. The models were evaluated using calibration, receiver operating characteristic (ROC), and decision curve analyses. Results: Age, sex, stroke history, diabetes, baseline mRS, baseline National Institutes of Health Stroke Scale score, and radiomics score were independent predictors of AIS outcomes. The area under the ROC curve of the clinical-radiomics model was 0.868 (95% confidence interval, 0.825-0.910) in the training cohort and 0.890 (0.844-0.936) in the validation cohort, which was significantly larger than that of the clinical or radiomics models. The clinical radiomics nomogram was well calibrated (p > 0.05). The decision curve analysis indicated its clinical usefulness. Conclusion: The clinical-radiomics model outperformed individual clinical or radiomics models and achieved satisfactory performance in predicting AIS outcomes.

Quality of Radiomics Research on Brain Metastasis: A Roadmap to Promote Clinical Translation

  • Chae Jung Park;Yae Won Park;Sung Soo Ahn;Dain Kim;Eui Hyun Kim;Seok-Gu Kang;Jong Hee Chang;Se Hoon Kim;Seung-Koo Lee
    • Korean Journal of Radiology
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    • 제23권1호
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    • pp.77-88
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    • 2022
  • Objective: Our study aimed to evaluate the quality of radiomics studies on brain metastases based on the radiomics quality score (RQS), Transparent Reporting of a multivariable prediction model for Individual Prognosis Or Diagnosis (TRIPOD) checklist, and the Image Biomarker Standardization Initiative (IBSI) guidelines. Materials and Methods: PubMed MEDLINE, and EMBASE were searched for articles on radiomics for evaluating brain metastases, published until February 2021. Of the 572 articles, 29 relevant original research articles were included and evaluated according to the RQS, TRIPOD checklist, and IBSI guidelines. Results: External validation was performed in only three studies (10.3%). The median RQS was 3.0 (range, -6 to 12), with a low basic adherence rate of 50.0%. The adherence rate was low in comparison to the "gold standard" (10.3%), stating the potential clinical utility (10.3%), performing the cut-off analysis (3.4%), reporting calibration statistics (6.9%), and providing open science and data (3.4%). None of the studies involved test-retest or phantom studies, prospective studies, or cost-effectiveness analyses. The overall rate of adherence to the TRIPOD checklist was 60.3% and low for reporting title (3.4%), blind assessment of outcome (0%), description of the handling of missing data (0%), and presentation of the full prediction model (0%). The majority of studies lacked pre-processing steps, with bias-field correction, isovoxel resampling, skull stripping, and gray-level discretization performed in only six (20.7%), nine (31.0%), four (3.8%), and four (13.8%) studies, respectively. Conclusion: The overall scientific and reporting quality of radiomics studies on brain metastases published during the study period was insufficient. Radiomics studies should adhere to the RQS, TRIPOD, and IBSI guidelines to facilitate the translation of radiomics into the clinical field.