• Title/Summary/Keyword: method validation #5

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Identification of Pb-Zn ore under the condition of low count rate detection of slim hole based on PGNAA technology

  • Haolong Huang;Pingkun Cai;Wenbao Jia;Yan Zhang
    • Nuclear Engineering and Technology
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    • v.55 no.5
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    • pp.1708-1717
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    • 2023
  • The grade analysis of lead-zinc ore is the basis for the optimal development and utilization of deposits. In this study, a method combining Prompt Gamma Neutron Activation Analysis (PGNAA) technology and machine learning is proposed for lead-zinc mine borehole logging, which can identify lead-zinc ores of different grades and gangue in the formation, providing real-time grade information qualitatively and semi-quantitatively. Firstly, Monte Carlo simulation is used to obtain a gamma-ray spectrum data set for training and testing machine learning classification algorithms. These spectra are broadened, normalized and separated into inelastic scattering and capture spectra, and then used to fit different classifier models. When the comprehensive grade boundary of high- and low-grade ores is set to 5%, the evaluation metrics calculated by the 5-fold cross-validation show that the SVM (Support Vector Machine), KNN (K-Nearest Neighbor), GNB (Gaussian Naive Bayes) and RF (Random Forest) models can effectively distinguish lead-zinc ore from gangue. At the same time, the GNB model has achieved the optimal accuracy of 91.45% when identifying high- and low-grade ores, and the F1 score for both types of ores is greater than 0.9.

Comparison of Marker Components and Biological Activities of Gamiguibi-tang(Jiaweiguipi-tang) Decoction and Commercial Extract Granules (가미귀비탕 탕액과 시판제제의 성분 및 생리활성 비교)

  • Kim, Jung Ok;Baek, Ka Yeon;Lee, Hwa Dong
    • Journal of Physiology & Pathology in Korean Medicine
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    • v.32 no.5
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    • pp.333-340
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    • 2018
  • Gamiguibi-tang (GGBT) is a traditional herbal medicine generally used to treat anemia, insomnia, anxiety, and nervousness. GGBT is being commercially produced in the form of extract granule and the quality control methods are specified in the Korean Herbal Pharmacopeia (KHP). However, there is no method to simultaneously analyze compound preparations. In this study, a HPLC method was developed and validated for the simultaneous determination of marker compounds in GGBT. And the contents of marker components and biological activities of the commercial GGBT extract granules (GGBT-2 and GGBT-3) were compared with those of the GGBT decoction (GGBT-1). We confirmed the robustness of simultaneous analytical method by monitoring the contents of the commercial GGBT products and carrying out validation. The marker components of GGBT were geniposide ($8.03{\sim}12.70{\mu}g/mL$), paeoniflorin ($2.79{\sim}4.25{\mu}g/mL$) and glycyrrhizic acid ($5.06{\sim}6.30{\mu}g/mL$). DPPH and ABTS radical scavenging activities were 47.34~63.17% and 21.52~33.61% in the GGBT products concentration of $1,000{\mu}g/mL$, respectively. The GGBT products significantly decreased NO, iNOS and COX-2 production in lipopolysaccharide (LPS)-induced RAW 264.7 macrophages in a concentration-dependent manner. The GGBT-2 had higher contents of marker components and biological activities than GGBT-1 and GGBT-3. The research suggest that be used in developing quality control methods for enhancing the quality of herbal medicines.

Determiniation and Validation of Alibendol using High Pressure Liquid Chromatography in Human plasma (고속액체크로마토그라피법을 이용한 사람 혈장 중 알리벤돌(Alibendol)의 정량 및 검증)

  • Song, Hyun-Ho;Yu, Ji-Young;Kim, Bo-Gyeom;Park, Hyeon-Ju;Choi, Kwang-Sik;Kwon, Young-Ee
    • YAKHAK HOEJI
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    • v.54 no.4
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    • pp.295-299
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    • 2010
  • The aim of this study was to develop and validate for determination of alibendol in human plasma by HPLC method. After precipitation of 500 ${\mu}l$ plasma samples by 50% methanol 50 ${\mu}l$ and 60% perchloric acid 30 ${\mu}l$ and the supernatant 50 ${\mu}l$ was injected into HPLC. The assay was performed isocratically using 10 mM potassium phosphate (pH 3.0) and acetonitrile (80 : 20, v/v) as mobile phase. The $C_{18}$ column (particle size $3.5{\mu}m$, $4.6{\times}50$ mm, Zorbax Eclipse) was used as a solid phase. The mobile phase was delivered at a flow-rate of 1.7 ml/min, detection was by ultraviolet absorption at 232 nm and concentrations were calculated on the basis of peak areas. In these conditions, alibendol can be separated from ethylparaben, the internal standard, and endogenous substances. The retention times of alibendol and ethylparaben were just about 2.6 and 3.5 minutes, respectively. This rapid HPLC method was validated by examining the precision and accuracy for inter- and intra-day analysis. The standard curve was linear ($R^2$=1.0000) over the concentration range of 0.05~20 ${\mu}g$/ml. The inter-day relative standard deviation (R.S.D.) and accuracy were 0.2~12.2% and 94.4~101.2% (82.7% at the lower limit of quatitation). The intra-day R.S.D. and accuracy were 0.1~11.8% and 98.8~102.5%, respectively. The method was successfully applied to the determination of alibendol in plasma for a pharmacokinetic study.

Analysis Method Development for Bound-MCPD (3-MCPD 지방산에스테르 분석법)

  • Woo, Sung-Min;Oh, Jae-Ho;Jang, Young-Mi;Kim, Mee-Hye
    • Journal of Food Hygiene and Safety
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    • v.25 no.4
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    • pp.294-302
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    • 2010
  • Toxicity of 3-MCPD that comes from food manufacture and processing is well-known. Recent studies reported that 3-MCPD fatty acid ester which is formed by metabolic material was 10~2000 times as much as 3-MCPD in food. This study made analysis method of 3-MCPD fatty acid esters by recent research and laboratory work, and determined the content of 3-MCPD and 3-MCPD fatty acid esters in sources and meat processing products. 3-MCPD fatty acid esters were analysed by GC/MS, which were hydrolyzed from fatty acid and then transferred 3-MCPD was extracted and reacted with derivative subject. As a result of analysis method validation, LOD was 5.4ppb, LOQ was 9.0ppb.

DETERMINATION OF MOISTURE AND NITROGEN ON UNDRIED FORAGES BY NEAR INFRARED REFLECTANCE SPECTROSCOPY(NIRS)

  • Cozzolino, D.;Labandera, M.;Inia La Estanzuela
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1620-1620
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    • 2001
  • Forages, both grazed and conserved, provide the basis of ruminant production systems throughout the world. More than 90 per cent of the feed energy consumed by herbivorous animals world - wide were provided by forages. With such world - wide dependence on forages, the economic and nutritional necessity of been able to characterize them in a meaningful way is vital. The characterization of forages for productive animals is becoming important for several reasons. Relative to conventional laboratory procedures, Near Infrared Reflectance Spectroscopy (NIRS) offers advantages of simplicity, speed, reduced chemical waste, and more cost-effective prediction of product functionality. NIR spectroscopy represents a radical departure from conventional analytical methods, in that entire sample of forage is characterized in terms of its absorption properties in the near infrared region, rather than separate subsamples being treated with various chemicals to isolate specific components. This forces the analyst to abandon his/her traditional narrow focus on the sample (one analyte at a time) and to take a broader view of the relationship between components within the sample and between the sample and the population from which it comes. forage is usually analysed by NIRS in dry and ground presentation. Initial success of NIRS analysis of coarse forages suggest a need to better understand the potential for analysis of minimally processed samples. Preparation costs and possible compositional alterations could be reduced by samples presented to the instrument in undried and unground conditions. NIRS has gained widespread acceptance for the analysis of forage quality constituents on dry material, however little attention has been given to the use of NIRS for chemical determinations on undried and unground forages. Relatively few works reported the use of NIRS to determine quality parameters on undried materials, most of them on both grass and corn silage. Only two works have been found on the determination of quality parameters on fresh forages. The objectives of this paper were (1) to evaluate the use of NIRS for determination of nitrogen and moisture on undried and unground forage samples and (2) to explore two mathematical treatments and two NIR regions to predict chemical parameters on fresh forage. Four hundred forage samples (n: 400) were analysed in a NIRS 6500 instrument (NIR Systems, PA, USA) in reflectance mode. Two mathematical treatments were applied: 1,4,4,1 and 2,5,5,2. Predictive equations were developed using modified partial least squares (MPLS) with internal cross - validation. Coefficient of determination in calibration (${R^2}_{CAL}$) and standard error in cross-validation (SECV) for moisture were 0.92 (12.4) and 0.92 (12.4) for 1,4,4,1 and 2,5,5,2 respectively, on g $kg^{-1}$ dry weight. For crude protein NIRS calibration statistics yield a (${R^2}_{CAL}$) and (SECV) of 0.85 (19.8) and 0.85 (19.6) for 1,4,4,1 and 2,5,5,2 respectively, on a dry weight. It was concluded that NIRS is a suitable method to predict moisture and nitrogen on fresh forage without samples preparation.

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Development and Validation of an HPLC-PDA Method for Quantitation of Ten Marker Compounds from Eclipta prostrata (L.) and Evaluation of Their Protein Tyrosine Phosphatase 1B, α-Glucosidase, and Acetylcholinesterase Inhibitory Activities

  • Nguyen, Duc Hung;Le, Duc Dat;Ma, Eun Sook;Min, Byung Sun;Woo, Mi Hee
    • Natural Product Sciences
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    • v.26 no.4
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    • pp.326-333
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    • 2020
  • The aerial parts of Eclipta prostrata is used as a traditional medicine and vegetable. In traditional folk medicine, it is used for treatment of hemorrhages, hepatic, disease, renal injuries, hair loss, tooth mobility, and viper bites. In this study, ten compounds (1 - 10) were isolated from the aerial parts of E. prostrata. A reliable high performance liquid chromatography equipped with photometric diode array detector (HPLC-PDA) method was developed to simultaneously quantitate 10 marker compounds [chlorogenic acid (1), paratensein 7-O-��-ᴅ-glucoside (2), quercetin 7-O-��-ᴅ-glucoside (3), luteolin 7-O-��-ᴅ-glucoside (4), apigenin 7-O-��-ᴅ-glucoside (5), apigenin 4'-O-��-ᴅ-glucoside (6), apigenin (7), luteolin (8), wedelolactone (9), and paratensein (10)]. In addition, compounds 5 and 6 showed considerable inhibitory effects against protein-tyrosine phosphatase 1B (PTP1B) enzyme. Moreover, compounds 6 - 8, and 10 exhibited potent α-glucosidase inhibitory effects with IC50 values of 24.5 ± 1.9, 33.0 ± 0.5, 45.5 ± 0.1, and 23.8 ± 1.0 µM, respectively. All compounds (1 - 10) showed considerable acetylcholinesterase (AChE) inhibitory effects with IC50 ranging from 30.1 to 75.2 µM.

Validation of Trienzyme Extraction-Microplate Assay for Folate in Korean Ancestral Rite Food (Trienzyme Extraction-Microplate Assay를 이용한 한국 차례 및 제사 음식의 엽산 분석 및 검증)

  • Park, Su-Jin;Jeong, Beom-Gyun;Jung, Jae Eun;Kim, Hyeon-Young;Jung, Gil-Rak;Hwang, Eun-Jung;Yoon, Sung-Won;Hyun, Taisun;Lee, Junsoo;Chun, Jiyeon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.5
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    • pp.716-724
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    • 2015
  • Trienzyme extraction coupled with microplate assay (Lactobacillus casei subsp. rhamnosus) was validated and applied for the determination of folate (vitamin B9) in Korean ancestral rite foods. Foods included five Guk (Tang), eleven Sookchaes, eight Jeoks, nine Jeons, six Jjims, and twenty desserts. Folate was detected in all samples: Guk (Tang) 4.62~18.84, Sookchae 6.13~48.40, Jeok 5.49~49.50, Jeon 6.96~30.77, Jjim 10.34~38.88, and desserts $3.33{\sim}49.55{\mu}g/100g$. The lowest folate content was observed in Sikhye ($3.33{\mu}g/100g$), whereas the highest was observed in Songhwa-dasik ($49.55{\mu}g/100g$). Folate analyses of certified reference materials, BCR-121 (whole meal flour) and BCR-487 (pig liver), showed good recoveries of 90.0% (0.45 mg/kg) and 92.4% (12.3 mg/kg), respectively. The recoveries (96.0 to 106.2%) obtained by analyzing eight spiked samples with different matrices also showed good accuracy. Both repeatability and reproducibility were less than 5%, indicating good precision. The quality control chart (n>30) obtained by running commercial folate fortified-wheat flour once a week for about 10 months showed that all assays were under control. All validation method and analytical quality control results showed that folate contents in Korean ancestral rite foods produced by microplate assay were reliable enough to be used for the construction of a national folate database.

Development & Validation of a Checklist for Infant and Child Developmental Screening (영유아 발달선열검사를 위한 체크리스트 개발 및 타당도 검정)

  • Ju, Hyeon-Ok;Lee, Nae-Young;Park, In-Sook;Lee, Sun-Ok;Kim, So-Hee
    • Child Health Nursing Research
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    • v.15 no.1
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    • pp.34-41
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    • 2009
  • Purpose: In this study, a Checklist for Infant and Child Developmental Screening (CICDS) was designed for use by primary pediatric health care providers to identify infants and children with developmental delays. Method: Each Item of the CICDS was constructed referring to existing tools. In 5 public health centers of B city, 500 infants and children were selected at the age of 2, 4, 6, 12, & 18 months and assessed between October and December 2006, CICDS and the Korea Denver II were compared to assesses the validity of the CICDS. Results: The CICDS consisted of 30 items in 4 areas; Personal-social, Fine motor-adaptive, Language, Gross motor. The results of the CICDS correlated significantly with the result of Korea Denver II at each month of age. (r=0.19; p<.01). Of the 500 infants and children, 148 were "suspect" for development delays (sensitivity of 96%, specificity 73%). On the CICDS, 74.6% of children received same result as Denver II. In discriminant analysis, 89.9% of children were identified correctly by CICDS (p<.01). Conclusion: CICDS could be a screening procedures to quickly and reliably identify infants with developmental delays. It also provides a mean of recording measurements of development characteristics.

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Validation of housekeeping genes as candidate internal references for quantitative expression studies in healthy and nervous necrosis virus-infected seven-band grouper (Hyporthodus septemfasciatus)

  • Krishnan, Rahul;Qadiri, Syed Shariq Nazir;Kim, Jong-Oh;Kim, Jae-Ok;Oh, Myung-Joo
    • Fisheries and Aquatic Sciences
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    • v.22 no.12
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    • pp.28.1-28.8
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    • 2019
  • Background: In the present study, we evaluated four commonly used housekeeping genes, viz., actin-β, elongation factor-1α (EF1α), acidic ribosomal protein (ARP), and glyceraldehyde 3-phosphate dehydrogenase (GAPDH) as internal references for quantitative analysis of immune genes in nervous necrosis virus (NNV)-infected seven-band grouper, Hyporthodus septemfasciatus. Methods: Expression profiles of the four genes were estimated in 12 tissues of healthy and infected seven-band grouper. Expression stability of the genes was calculated using the delta Ct method, BestKeeper, NormFinder, and geNorm algorithms. Consensus ranking was performed using RefFinder, and statistical analysis was done using GraphpadPrism 5.0. Results: Tissue-specific variations were observed in the four tested housekeeping genes of healthy and NNV-infected seven-band grouper. Fold change calculation for interferon-1 and Mx expression using the four housekeeping genes as internal references presented varied profiles for each tissue. EF1α and actin-β was the most stable expressed gene in tissues of healthy and NNV-infected seven-band grouper, respectively. Consensus ranking using RefFinder suggested EF1α as the least variable and highly stable gene in the healthy and infected animals. Conclusions: These results suggest that EF1α can be a fairly better internal reference in comparison to other tested genes in this study during the NNV infection process. This forms the pilot study on the validation of reference genes in Hyporthodus septemfasciatus, in the context of NNV infection.

Effect of Sample Preparation on Prediction of Fermentation Quality of Maize Silages by Near Infrared Reflectance Spectroscopy

  • Park, H.S.;Lee, J.K.;Fike, J.H.;Kim, D.A.;Ko, M.S.;Ha, Jong Kyu
    • Asian-Australasian Journal of Animal Sciences
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    • v.18 no.5
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    • pp.643-648
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    • 2005
  • Near infrared reflectance spectroscopy (NIRS) has become increasingly used as a rapid, accurate method of evaluating some chemical constituents in cereal grains and forages. If samples could be analyzed without drying and grinding, then sample preparation time and costs may be reduced. This study was conducted to develop robust NIRS equations to predict fermentation quality of corn (Zea mays) silage and to select acceptable sample preparation methods for prediction of fermentation products in corn silage by NIRS. Prior to analysis, samples (n = 112) were either oven-dried and ground (OD), frozen in liquid nitrogen and ground (LN) and intact fresh (IF). Samples were scanned from 400 to 2,500 nm with an NIRS 6,500 monochromator. The samples were divided into calibration and validation sets. The spectral data were regressed on a range of dry matter (DM), pH and short chain organic acids using modified multivariate partial least squares (MPLS) analysis that used first and second order derivatives. All chemical analyses were conducted with fresh samples. From these treatments, calibration equations were developed successfully for concentrations of all constituents except butyric acid. Prediction accuracy, represented by standard error of prediction (SEP) and $R^2_{v}$ (variance accounted for in validation set), was slightly better with the LN treatment ($R^2$ 0.75-0.90) than for OD ($R^2$ 0.43-0.81) or IF ($R^2$ 0.62-0.79) treatments. Fermentation characteristics could be successfully predicted by NIRS analysis either with dry or fresh silage. Although statistical results for the OD and IF treatments were the lower than those of LN treatment, intact fresh (IF) treatment may be acceptable when processing is costly or when possible component alterations are expected.