• Title/Summary/Keyword: Calibration Standard

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

  • Yu, Young-Beob;Kim, Mi-Jung;Huang, Dae Sun;Ha, Hye-Kyeong;Ma, Jin-Yeul;Shin, Hyeun-Kyoo
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.331-338
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    • 2007
  • Licorice, Glycyrrhizae Radix is widely used as a herbal medicines and a dietary supplements in East Asia. We employed high performance liquid chromatography electrospray ionization tandem mass spectrometry to determine liquiritin and glycyrrhizin in the Glycyrrhizae Radix. Liquiritin and glycyrrhizin in Glycyrrhizae Radix were ionized by positive ion pneumatically assisted electrospray and detected by HPLC-MS/MS in the multiple-reaction monitoring (MRM) mode using precursor ${\rightarrow}$ product ion combinations at m/z $436.2{\rightarrow}257.0$ and $823.4{\rightarrow}453.4$, respectively. The assay had a calibration range from 10 to 3,000 ng/mL. The limits of detection (LOD) of the liquiritin and glycyrrhizin were 0.4 ng/mL and 0.01 ng/mL, respectively. The reproducibility and repeatability (relative standard deviation) at different analyte concentrations varied from 103 to 113 % and 0.95 to 1.8 %, respectively. According to the above results, HPLC-MS/MS method permits assignment of tentative structures such as liquiritin and glycyrrhizin in the Glycyrrhizae Radix.

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

  • Lee, Geun Sang
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.30 no.5D
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    • pp.533-540
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    • 2010
  • Dam is very important facility in water supply and flood control. Therefore study needs to analyze reservoir capacity accurately to manage Dam efficiently. This study compared time series reservoir capacity using multi-dimensional spatial information to Chungju Dam reservoir and major conclusions are as follows. First, LiDAR and multi beam echo sounder survey were carried out in land zone and water zone of Dam reservoir area. And calibration process was performed to enhance the accuracy of survey data and it could be constructed that multi dimensional spatial information which was clearly satisfied with the standard of tolerance error by validation with ground control points. Reservoir capacity by water level was calculated using triangle irregular network from detailed topographic data that was constructed by linked with airborne LiDAR and multi beam echo sounder data, and curve equation of reservoir capacity was developed through regression analysis in 2008. In the comparison of the reservoir capacity of 2008 with those of 1986 and 1996, the higher water level goes, total reservoir capacity of 2008 showed decrease because of the increase of sediment in reservoir. Also, erosion and sediment area could be analyzed through calculating the reservoir capacity by the range of water level. Especially the range of water level as 130.0~135.0 which is the upper part of average water level, showed the highest erosion characteristics during 1986~2008 and 1996~2008 and it is considered that the erosion of reservoir slant by heavy rainfall is major reason.

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

  • Ye Ji Lee;Young Eun Kim;Jae Yong Seo;Hyun Dae Cho
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.49 no.4
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    • pp.291-298
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    • 2023
  • In this study, a quantitative analysis method was developed using high-performance liquid chromatography (HPLC) to analyze the content of ceramide NP in lotion, cream, and cleanser formulations in cosmetics. The analysis was performed using a C18 column, and the mobile phase was set at a ratio of 70 : 30 for acetonitrile and methanol, the flow rate was set to 0.8 mL/min, and the column temperature was set to 20 ℃. The method was verified by analyzing specificity, linearity, limit of detection, limit of quantitation, accuracy, and precision in accordance with the ICH guidelines. As a result of validating the method, the linearity of the calibration curve was excellent (R2 = 0.99984). The accuracy of the lotion, cream, and cleanser formulations was confirmed with a recovery rate ranging from 95.11% to 100.48%. The precision analysis showed a low relative standard deviation (RSD) of less than 0.26%. The limit of detection was 0.902 ㎍/mL, and the limit of quantitation was 2.733 ㎍/mL. Through this quantitative analysis method of ceramide NP applied in cosmetics, it is expected to assist in the quality control of products by enabling measurement even when it is difficult to separate the main peak due to the influence of interfering substances.

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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    • v.23 no.8
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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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    • v.23 no.1
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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.

Analysis of Systemic Pesticide Imidacloprid and Its Metabolites in Pepper using QuEChERS and LC-MS/MS (QuEChERS 전처리와 LC-MS/MS를 이용한 고추 중 침투성농약 Imidacloprid 및 대사물질 동시분석법)

  • Seo, Eun-Kyung;Kim, Taek-Kyum;Hong, Su-Myeong;Kwon, Hye-Yong;Kwon, Ji-Hyung;Son, Kyung-Ae;Kim, Jang-Eok;Kim, Doo-Ho
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.264-270
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    • 2013
  • Imidacloprid is a systemic insecticide which act as an insect neurotoxin. It used for control of pest such as aphids and other sucking insects in fruits and vegetables. Systemic pesticides move inside a crop following absorption by the plant, and these were converted into a variety of metabolites. Sometimes these metabolites make a problem about safety of agricultural products. So a simultaneous determination method of pesticide and its metabolites is needed, to monitor their presence in agricultural product and study on the fate of pesticide in a plant. This study's aim is to investigate simultaneous analysis method of imidacloprid and its metabolites, imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, and 6-chloronicotinic acid in red pepper using QuEChERS method and LC-MS/MS systems. QuEChERS method was modifed beacuase $MgSO_4$ salts decreased the recoveries of 6-chloronicotinic acid in extraction procedure. Imidacloprid and its metabolites were extracted by acetonitrile with 1% glacial acetic acid and the extracts were purified through QuEChERS with primary secondary amine (PSA) and $C_{18}$ and analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.999. Recovery studies were carried out on spiked pepper blank sample at four concentration levels (0.01, 0.04 and 0.1, 0.4 mg/kg). The average recoveries of imidacloprid and its metabolites were in the range of 70~120% with < 20% RSD. This result indicated that the method using QuEChERS and LC-MS/MS was suitable for the simultaneous determination of imidacloprid and its metabolites in red pepper.

DISEASE DIAGNOSED AND DESCRIBED BY NIRS

  • Tsenkova, Roumiana N.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1031-1031
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    • 2001
  • The mammary gland is made up of remarkably sensitive tissue, which has the capability of producing a large volume of secretion, milk, under normal or healthy conditions. When bacteria enter the gland and establish an infection (mastitis), inflammation is initiated accompanied by an influx of white cells from the blood stream, by altered secretory function, and changes in the volume and composition of secretion. Cell numbers in milk are closely associated with inflammation and udder health. These somatic cell counts (SCC) are accepted as the international standard measurement of milk quality in dairy and for mastitis diagnosis. NIR Spectra of unhomogenized composite milk samples from 14 cows (healthy and mastitic), 7days after parturition and during the next 30 days of lactation were measured. Different multivariate analysis techniques were used to diagnose the disease at very early stage and determine how the spectral properties of milk vary with its composition and animal health. PLS model for prediction of somatic cell count (SCC) based on NIR milk spectra was made. The best accuracy of determination for the 1100-2500nm range was found using smoothed absorbance data and 10 PLS factors. The standard error of prediction for independent validation set of samples was 0.382, correlation coefficient 0.854 and the variation coefficient 7.63%. It has been found that SCC determination by NIR milk spectra was indirect and based on the related changes in milk composition. From the spectral changes, we learned that when mastitis occurred, the most significant factors that simultaneously influenced milk spectra were alteration of milk proteins and changes in ionic concentration of milk. It was consistent with the results we obtained further when applied 2DCOS. Two-dimensional correlation analysis of NIR milk spectra was done to assess the changes in milk composition, which occur when somatic cell count (SCC) levels vary. The synchronous correlation map revealed that when SCC increases, protein levels increase while water and lactose levels decrease. Results from the analysis of the asynchronous plot indicated that changes in water and fat absorptions occur before other milk components. In addition, the technique was used to assess the changes in milk during a period when SCC levels do not vary appreciably. Results indicated that milk components are in equilibrium and no appreciable change in a given component was seen with respect to another. This was found in both healthy and mastitic animals. However, milk components were found to vary with SCC content regardless of the range considered. This important finding demonstrates that 2-D correlation analysis may be used to track even subtle changes in milk composition in individual cows. To find out the right threshold for SCC when used for mastitis diagnosis at cow level, classification of milk samples was performed using soft independent modeling of class analogy (SIMCA) and different spectral data pretreatment. Two levels of SCC - 200 000 cells/$m\ell$ and 300 000 cells/$m\ell$, respectively, were set up and compared as thresholds to discriminate between healthy and mastitic cows. The best detection accuracy was found with 200 000 cells/$m\ell$ as threshold for mastitis and smoothed absorbance data: - 98% of the milk samples in the calibration set and 87% of the samples in the independent test set were correctly classified. When the spectral information was studied it was found that the successful mastitis diagnosis was based on reviling the spectral changes related to the corresponding changes in milk composition. NIRS combined with different ways of spectral data ruining can provide faster and nondestructive alternative to current methods for mastitis diagnosis and a new inside into disease understanding at molecular level.

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Improvement of Radar Rainfall Estimation Using Radar Reflectivity Data from the Hybrid Lowest Elevation Angles (혼합 최저고도각 반사도 자료를 이용한 레이더 강우추정 정확도 향상)

  • Lyu, Geunsu;Jung, Sung-Hwa;Nam, Kyung-Yeub;Kwon, Soohyun;Lee, Cheong-Ryong;Lee, Gyuwon
    • Journal of the Korean earth science society
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    • v.36 no.1
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    • pp.109-124
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    • 2015
  • A novel approach, hybrid surface rainfall (KNU-HSR) technique developed by Kyungpook Natinal University, was utilized for improving the radar rainfall estimation. The KNU-HSR technique estimates radar rainfall at a 2D hybrid surface consistings of the lowest radar bins that is immune to ground clutter contaminations and significant beam blockage. Two HSR techniques, static and dynamic HSRs, were compared and evaluated in this study. Static HSR technique utilizes beam blockage map and ground clutter map to yield the hybrid surface whereas dynamic HSR technique additionally applies quality index map that are derived from the fuzzy logic algorithm for a quality control in real time. The performances of two HSRs were evaluated by correlation coefficient (CORR), total ratio (RATIO), mean bias (BIAS), normalized standard deviation (NSD), and mean relative error (MRE) for ten rain cases. Dynamic HSR (CORR=0.88, BIAS= $-0.24mm\;hr^{-1}$, NSD=0.41, MRE=37.6%) shows better performances than static HSR without correction of reflectivity calibration bias (CORR=0.87, BIAS= $-2.94mm\;hr^{-1}$, NSD=0.76, MRE=58.4%) for all skill scores. Dynamic HSR technique overestimates surface rainfall at near range whereas it underestimates rainfall at far ranges due to the effects of beam broadening and increasing the radar beam height. In terms of NSD and MRE, dynamic HSR shows the best results regardless of the distance from radar. Static HSR significantly overestimates a surface rainfall at weaker rainfall intensity. However, RATIO of dynamic HSR remains almost 1.0 for all ranges of rainfall intensity. After correcting system bias of reflectivity, NSD and MRE of dynamic HSR are improved by about 20 and 15%, respectively.

Development and Validation of an Analytical Method for Determination of Fungicide Benzovindiflupyr in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 벤조빈디플루피르의 잔류시험법 개발 및 검증)

  • Lim, Seung-Hee;Do, Jung-Ah;Park, Shin-Min;Pak, Won-Min;Yoon, Ji Hye;Kim, Ji Young;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.298-305
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    • 2017
  • Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.

A comparison study of 76Se, 77Se and 78Se isotope spikes in isotope dilution method for Se (셀레늄의 동위원소 희석분석법에서 첨가 스파이크 동위원소 76Se, 77Se 및 78Se들의 비교분석)

  • Kim, Leewon;Lee, Seoyoung;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.170-178
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    • 2016
  • Accuracy and precision of ID methods for different spike isotopes of 76Se, 77Se, and 78Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and 78Se showed was a bit better than 76Se and 77Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for 78Se, 76Se and 77Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of 78Se isotope spike (over 100 % RSD). 76Se and 77Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, 78Se should be avoided when large amount of Br exists in matrix. Either 76Se or 77Se would provide accurate results.