• Title/Summary/Keyword: precision validation

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Multi-block PCA for Sensor Fault Detection and Diagnosis of City Gas Network (도시가스 배관망의 고장 탐지 및 진단을 위한 다중블록 PCA 적용 연구)

  • Yeon-ju Baek;Tae-Ryong Lee;Jong-Seun Kim;Hong-Cheol Ko
    • Journal of the Korean Institute of Gas
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    • v.28 no.2
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    • pp.38-46
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    • 2024
  • The city gas pipeline network is characterized by being widely distributed and hierarchically connected in a complex manner over a wide area. In order to monitor the status of the widely distributed network pressures with high precision, Multi-block PCA(MBPCA) is recommended. However, while MBPCA has excellent performance in identifying faulty sensors as the number of sensors increases, the fault detection performance deteriorates, and also there is a problem that the model needs to be updated entirely even if minor changes occur. In this study, we developed fault detectability index and fault identificability index to determine the effectiveness of MBPCA application block by block. Based on these indices, we distinguished MBPCA and PCA blocks and developed a fault detection and diagnostic system for the city gas pipeline network of Haean Energy Co., Ltd., and were able to solve the problems that arise when there are many sensors.

Simultaneous Analysis Method for 27 Endocrine Disrupting Chemicals in Human Urine using UPLC-MS/MS (UPLC-MS/MS를 이용한 소변 시료 중 내분비계 교란물질 27종 동시분석법 확립)

  • Subeen Park;Na-youn Park;Younglim Kho
    • Journal of the Korean Chemical Society
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    • v.68 no.4
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    • pp.191-198
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    • 2024
  • Endocrine disrupting chemicals (EDCs) are compounds that come from outside the body and disrupt hormone action within the body's endocrine system. Examples include parabens, benzophenones, bisphenols, and phthalates, which are currently used in a wide range of applications. However, continuous exposure to them can have negative effects on glycemic control, reproduction, metabolism, nervous system development, pregnancy, childbirth, and growth. In this study, human samples (urine) were pretreated using liquid-liquid-extraction to determine the exposure level of EDCs and then analyzed effectively and rapidly by UPLC-MS/MS. In this way, the analytical conditions were established and the reliability of the simultaneous analysis method was evaluated through method validation. The results showed that the accuracy ranged from 75.28 to 122.36% and the precision ranged from 2.16 to 22.74%. The analytical method established in this study can be used as a methodology for future studies to evaluate and monitor the exposure of EDCs in human samples.

Development and Validation of Analytical Method for Wogonin, Quercetin, and Quercetin-3-O-glucuronide in Extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus Mixture (연잎, 상엽, 건조 무 혼합 추출물의 지표성분 wogonin, quercetin 및 quercetin-3-O-glucuronide의 분석법 개발 및 검증)

  • Jang, Gill-Woong;Park, Eun-Young;Choi, Seung-Hyun;Choi, Sun-il;Cho, Bong-Yeon;Sim, Wan-Sup;Han, Xinggao;Cho, Hyun-Duk;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.289-295
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    • 2018
  • The aim of this study was to develop and validate an analytical method for determining the presence of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for wogonin, quercetin, and quercetin-3-O-glucuronide using high performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for wogonin, quercetin, and quercetin-3-O-glucuronide were 0.9999. The LOD for wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.09 to 0.16 and those for the LOQ ranged from 0.26 to $0.48{\mu}g/mL$. The inter-day and intra-day precision values of wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.74 to 1.87 and from 0.28 to 1.12%, respectively. The inter-day and intra-day accuracies were 99.96~115.88% and 99.73~114.81%, respectively. Therefore, the analytical method was validated for the detection of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures.

Validation of a Rapid Quantitative Method for the Residues of Nitrofuran Metabolites in Loach by Accelerated Solvent Extraction and HPLC Triple Quadrupole Mass Spectrometry

  • Ryu, Eun Chae;Han, Yun-jeong;Park, Seong-soo;Lim, Chul-joo;Choi, Sunok;Park, Se Chang
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.85-93
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    • 2016
  • A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

Method for Validation of Caffeoylquinic Acid Derivatives in Ligularia fischeri Leaf Extract as Functional Ingredients (건강기능식품 기능성 원료로서 곰취잎 추출물의 Caffeoylquinic Acid계 성분 분석법 검증)

  • Kwon, Jin Gwan;Kim, Jin Kyu;Seo, Changon;Hong, Seong Su;Ahn, Eun-Kyung;Seo, Dong-Wan;Oh, Joa Sub
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.1
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    • pp.61-67
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    • 2016
  • An HPLC analysis method was developed for standard determinations of chlorogenic acid, 3,4-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4,5-di-O-caffeoylquinic acid as functional health materials in Ligularia fischeri extract. HPLC was performed on a $C_{18}$ Kromasil column ($4.6{\times}250mm$, $5{\mu}m$ column) with a gradient elution of 0.1% (v/v) trifluoroacetic acid and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analytes were detected at 330 nm. The HPLC method was validated in accordance with the International Conference on Harmonization guideline of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation for the four compounds were 3.0~14.6 and $9.2{\sim}44.4{\mu}g/mL$, respectively. Calibration curves showed good linearity ($r^2$ > 0.999), and the precision of analysis was satisfied (less than 0.9%). Recoveries of quantified compounds ranged from 98.96 to 101.81%. This result indicates that the established HPLC method is very useful for the determination of marker compounds in Ligularia fischeri leaf extracts.

Establishment of Choline Analysis in Infant Formulas and Follow-up Formulas by Ion Chromatograph (이온크로마토그래프를 이용한 조제유류 및 영아용·성장기용 조제식 중 콜린 함량 분석법 연구)

  • Hwang, Kyung Mi;Ham, Hyeon Suk;Lee, Hwa Jung;Kang, Yoon Jung;Yoon, Hae Seong;Hong, Jin Hwan;Lee, Hyoun Young;Kim, Cheon Hoe;Oh, Keum Soon
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.411-417
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    • 2017
  • This study was conducted to establish the analysis method for the contents of choline in infant formulas and follow-up formulas by ion chromatograph (IC). To optimize the method, we compared several conditions for extraction, purification and instrumental measurement using spiked samples and certified reference material (CRM; NIST SRM 1849a) as test materials. IC method for choline was established using Ion Pac CG column and 18 mM $H_2SO_4$ mobile phase. The parameters of validation were specificity, linearity, LOD, LOQ, recovery, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity, $R_2$ was over 0.999 in range of 0.5~10 mg/L. The detection limit and quantification limit were 0.14, 0.43 mg/L. The accuracy and precision of this method using CRM were 95%, 2.1% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested products were acceptable contents of choline compared with component specification for nutrition labeling. The standard operating procedures were prepared for choline to provide experimental information and to strengthen the management of nutrient in infant formula and follow-up formula.

Development and Validation of Analytical Method for Determination of Biphenyl Analysis in Foods (식품 중 비페닐 분석법 개발 및 유효성 검증)

  • Kim, Jung-Bok;Kim, Myung-Chul;Song, Sung-Woan;Shin, Jae-Wook
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.4
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    • pp.459-464
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    • 2017
  • Biphenyl is used as an intermediate in the production of crop protection products, a solvent in pharmaceutical production, and as a component in the preservation of citrus fruits in many countries. Biphenyl is not authorized for use and also does not have standards or specifications as a food additive in Korea. National and imported food products are likely to contain biphenyl. Therefore, control and management of these products is required. In this study, a simple analytical method was developed and validated using HPLC to determine biphenyl in food. These methods are validated by assessing certain performance parameters: linearity, accuracy, precision, recovery, limit of detection (LOD), and limit of quantitation (LOQ). The calibration curve was obtained from 1.0 to $100.0{\mu}g/mL$ with satisfactory relative standard deviations (RSD) of 0.999 in the representative sample (orange). In the measurement of quality control (QC) samples, accuracy was in the range of 95.8~104.0% within normal values. The inter-day and inter-day precision values were less than 2.4% RSD in the measurement of QC samples. Recoveries of biphenyl from spiked orange samples ranged from 92.7 to 99.4% with RSD between 0.7 and 1.7% at levels of 10, 50, and $100{\mu}g/mL$. The LOD and LOQ were determined to be 0.04 and $0.13{\mu}g/mL$, respectively. These results show that the developed method is appropriate for biphenyl identification and can be used to examine the safety of citrus fruits and surface treatments containing biphenyl residues.

Development and Validation of Analytical Method and Antioxidant Effect for Berberine and Palmatine in P.amurense (황백의 지표성분 berberine과 palmatine의 분석법 개발과 검증 및 항산화 효능 평가)

  • Jang, Gill-Woong;Choi, Sun-Il;Han, Xionggao;Men, Xiao;Kwon, Hee-Yeon;Choi, Ye-Eun;Park, Byung-Woo;Kim, Jeong-Jin;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.35 no.6
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    • pp.544-551
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    • 2020
  • The aim of this study was to develop and validate a simultaneous analytical method for berberine and palmatine, which are representative substances of Phellodendron amurense, and to evaluate the antioxidant activity. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for berberine and palmatine using high-performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for berberine and palmatine exhibited 0.9999. The LODs for berberine and palmatine were 0.32 to 0.35 µg/mL and the LOQs were 0.97 to 1.06 µg/mL, respectively. The inter-day and intra-day precision values for berberine and palmatine were from 0.12 to 1.93 and 0.19 to 2.89%, respectively. The inter-day and intra-day accuracies were 98.43-101.45% and 92.39-100.60%, respectively. In addition, the simultaneous analytical method was validated for the detection of berberine and palmatine. Moreover, we conducted FRAP and NaNO2 scavenging activity assays to measure the antioxidant activities of berberine and palmatine, and both showed antioxidant activity. These results suggest that P.amurense could be a potential natural resource for antioxidant activity and that the efficacy can be confirmed by investigating the content of the berberine and palmatine.

Establishment of Analytical Methods for Melamine Related Compounds in Biological Samples (생체시료 중 멜라민 화합물의 미량분석법 개발연구)

  • Han, Kyoung-Moon;Kim, Jin-Ho;Cho, Soo-Yeul;Shim, Sun-Bo;Lee, Jin-Hee;Lee, Ji-Hyun;Hwang, In-Sun;Kim, Sung-Il;Cho, Yang-Ha;Chai, Gap-Yong;Kwon, Soon-Jae;Lee, Jun-Ho
    • Journal of Food Hygiene and Safety
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    • v.26 no.2
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    • pp.125-141
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    • 2011
  • Melamine has raised international concerns for its catastrophic health effects from tainted infant formula. This report concerns the developmental validation of a sensitive HPLC/MS/MS and GC/MS methods about melamine and cyanuric acid in human urine and serum. Analytical detection ranges of LC/MS was from 0.2 to 5.0 ng/mL and 2.0 to 60.0 ng/mL about melamine and cyanuric acid, respectively. The limits of quantification and confirmation are 0.2 ng/mL for both analytes in human urine and serum by LC/MS/MS. The range of recovery was 91.6%, and 107.6% for cyanuric acid and melamine in urine, respectively. The range of precision coefficient variation was from 2.0%, to 11.8% for cyanuric acid and melamine in urine. The range of recovery was from 94.9%, to 119.0% about cyanuric acid and melamine in serum, respectively. The range of precision coefficient variation from was 3.7%, and 13.5% about cyanuric acid and melamine in serum. Analytical detection ranges of GC/MS were 5.0 to 100.0 ng/mL about melamine and cyanuric acid, respectively. The limits of quantification and confirmation are 5.0 ng/mL for both analytes in human urine and serum by GC/MS. The range of recovery was from 83.7%, to 114.5% for cyanuric acid and melamine in urine, respectively. The range of precision coefficient variation was 3.5%, and 10.7% for cyanuric acid and melamine in urine. The range of recovery was 94.4%, and 110.7% for cyanuric acid and melamine in serum, respectively. The range of precision coefficient variation from was 3.9%, and 13.8% for cyanuric acid and melamine in serum. Several changes were taken to optimize performance by this method.

The Validation of a Commercial Testosterone RIA Test Kits (Testosterone RIA 검사 kit 별 유효성 비교평가)

  • Ryu, Hwa-jin;Shin, Seon-yeong;Cho, Seong-uk
    • The Korean Journal of Nuclear Medicine Technology
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    • v.26 no.1
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    • pp.38-41
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    • 2022
  • Purpose Testosterone is a steroid hormone synthesized by the Leydig cells of the testes in men, and by the adrenal cortex and ovaries in women. Testosterone production is regulated by luteinzing hormone secreted by the anterior pituitary gland. In this experiment, the effectiveness of testosterone radioimmunoassay (RIA) kits produced by three companies was evaluated and compared in case the production of testosterone kits was stopped or supply problems occurred. Materials and Methods In October 2021, samples were collected from the patients (n=49) who requested the testosterone RIA test. The experiment was conducted by dividing the patient's sample into low concentration (1.0 ng/mL or less), medium concentration (2.0-4.0 ng/mL) and high concentration (6.0 ng/mL or more). The Testosterone RIA test compared and evaluated the validity of Company A kits used in this hospital and those of Company B and C used in other hospitals. The precision, sensitivity, recovery, linearity and correlation were evaluated for each kit. The testosterone RIA test was carried out in accordance with the insert kit manual for each manufacturer. Results As a result of measuring the precision of the intra assay, the Coefficient of Variation (CV) value of the company A kit was high at 11.4% only in the low concentration sample, and in the case of the company B and C kits, the CV value was less than 10% at low, medium, and high concentrations. In the inter-assay precision measurement, the CV value was less than 15% in both A and C kits, but in the case of the B kit, the CV value exceeded 15% at low and medium concentrations. Sensitivity was 0.13 ng/mL for company A, 0.01 ng/mL for company B, and 0.01 ng/mL for company C, and the linearity of all three kits showed excellent linearity. In the case of recovery rate, all of the A, B, and C company kits showed results that were out of 90-110%. In the case of correlation test, when compared with the company A kit currently use in here, the correlation coefficient (R2) value for the company B kit was 0.9508, and for the company C kit was 0.9352 Conclusion As a result, there was a slight difference in precision at the low concentration sample. The correlation test showed an excellent correlation coefficient. However, it was difficult to secure samples of various concentrations because there were not many tests of testosterone requested at this hospital. So, additional experiments should be carried out by acquiring samples of various concentrations on each laboratory later.