• Title/Summary/Keyword: method validation #5

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Content Comparative Analysis and Classification for Piniellia ternate, P. pedatisecta and Typhonium flagelliforme by HPLC-PDA analysis (HPLC-PDA를 이용한 반하, 호장남성, 수반하의 분류 및 함량분석)

  • Jo, Ji Eun;Lee, A Yeong;Kim, Hyo Seon;Moon, Byeong Cheol;Choi, Goya;Ji, Yunui;Kim, Ho Kyoung
    • The Korea Journal of Herbology
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    • v.28 no.5
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    • pp.95-101
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    • 2013
  • Objectives : A quantitative method using high performance liquid chromatography with a photodiode array detector(HPLC-PDA) was established for the quantitative analysis of the four main compound and pattern analysis to classification Piiellia ternate, P. pedatisecta and Typhonium flagelliforme. Methods : The analytical procedure for the determination of P. ternata, together with the known main compounds uracil, uridine, guanosine and adenosine was established. Optimum HPLC-PDA separation of these P. ternata was possible on Luna C18(2) column material, using water and acetonitrile as mobile phase. The method was validated according to regulatory guidelines. In addition, this assay method were analyzed for the content of four main compound in P. ternata, P. pedatisecta and T. flagelliforme and by data obtained from the HPLC-PDA analysis was performed principal component analysis(PCA). Results : Validation results indicated that the HPLC method is well suited for the determination of the roots of P. ternata with a good linearity ($r^2$ > 0.999), precision and recovery rates. Analysis of HPLC-PDA, the average content of uracil, uridine, guanosine and adenosine was significantly higher in P. ternate>P. pedatisecta> T. flagelliforme order. The application of PCA to main compound data by HPLC-PDA permitted the effective discrimination among the three species. Conclusions : Analysis of both HPLC-PDA and PCA confirmed the fact that four main compound and pattern profiles of P. ternata, P. pedatisecta and T. flagelliforme were different from each other.

Multiclass Method for the Determination of Anthelmintic and Antiprotozoal Drugs in Livestock Products by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hyunjin Park;Eunjung Kim;Tae Ho Lee;Sihyun Park;Jang-Duck Choi;Guiim Moon
    • Food Science of Animal Resources
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    • v.43 no.5
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    • pp.914-937
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    • 2023
  • The objective of this study was to establish a multi-residue quantitative method for the analysis of anthelmintic and antiprotozoal drugs in various livestock products (beef, pork, and chicken) using ultra-high-performance liquid chromatography-tandem mass spectrometry. Each compound performed validation at three different levels i.e., 0.5, 1, and 2× the maximum residue limit according to the CODEX guidelines (CAC/GL 71-2009). This study was conducted according to the modified quick, easy, cheap, effective, rugged, and safe procedure. The matrix-matched calibrations gave correlation coefficients >0.98, and the obtained recoveries were in the range of 60.2%-119.9%, with coefficients of variation ≤32.0%. Furthermore, the detection and quantification limits of the method were in the ranges of 0.03-3.2 and 0.1-9.7 ㎍/kg, respectively. Moreover, a survey of residual anthelmintic and antiprotozoal drugs was also carried out in 30 samples of beef, pork, and chicken collected in Korea. Toltrazuril sulfone was detected in all three samples. Thus, our results indicated that the developed method is suitable for determining the anthelmintic and antiprotozoal drug contents in livestock products.

Estimation of reaction forces at the seabed anchor of the submerged floating tunnel using structural pattern recognition

  • Seongi Min;Kiwon Jeong;Yunwoo Lee;Donghwi Jung;Seungjun Kim
    • Computers and Concrete
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    • v.31 no.5
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    • pp.405-417
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    • 2023
  • The submerged floating tunnel (SFT) is tethered by mooring lines anchored to the seabed, therefore, the structural integrity of the anchor should be sensitively managed. Despite their importance, reaction forces cannot be simply measured by attaching sensors or load cells because of the structural and environmental characteristics of the submerged structure. Therefore, we propose an effective method for estimating the reaction forces at the seabed anchor of a submerged floating tunnel using a structural pattern model. First, a structural pattern model is established to use the correlation between tunnel motion and anchor reactions via a deep learning algorithm. Once the pattern model is established, it is directly used to estimate the reaction forces by inputting the tunnel motion data, which can be directly measured inside the tunnel. Because the sequential characteristics of responses in the time domain should be considered, the long short-term memory (LSTM) algorithm is mainly used to recognize structural behavioral patterns. Using hydrodynamics-based simulations, big data on the structural behavior of the SFT under various waves were generated, and the prepared datasets were used to validate the proposed method. The simulation-based validation results clearly show that the proposed method can precisely estimate time-series reactions using only acceleration data. In addition to real-time structural health monitoring, the proposed method can be useful for forensics when an unexpected accident or failure is related to the seabed anchors of the SFT.

Validation of new saliva test using SALIgAE® (사건현장 검사를 위해 변형된 SALIgAE® 타액검사법의 유효성 검토)

  • Lim, Si-Keun;Kwak, Kyung-Don;Choi, Dong-Ho;Han, Myun-Soo
    • Analytical Science and Technology
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    • v.21 no.1
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    • pp.48-52
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    • 2008
  • A new forensic saliva test method using $SALIgAE^{(R)}$ was evaluated in this study. The sensitivity and specificity of $SALIgAE^{(R)}$ were examined and compared to those of other saliva test methods such as agarose gel diffusion method and $Phadebas^{(R)}$ test sheet method. $SALIgAE^{(R)}$ showed high sensitivity and specificity to human saliva in addition to quickness. Moreover modified $SALIgAE^{(R)}$ method was cheap and easy to use in crime scene and DNA laboratory. $SALIgAE^{(R)}$ was very stable at room temperature and had no effect on STR typing.

Validation of method for chemical treatment of pig carcasses for the control of livestock infectious diseases (가축 전염병 관리를 위한 돼지 사체의 화학적 처리 방법)

  • Oh, Yeonsu;Yoon, Suk Hoon;Tark, Dong-Seob;Cho, Ho-Seong
    • Korean Journal of Veterinary Service
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    • v.44 no.4
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    • pp.283-290
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    • 2021
  • This is a study on the improvement of the chemical treatment method of the livestock carcass treatment newly introduced in the livestock infectious disease prevention method in order to improve the problems of the existing burial-centered carcass treatment method when a livestock infectious disease occurs. It was conducted to establish detailed treatment standards for the chemical treatment method of pig carcasses based on the results of proof of the absence of infectious diseases in pigs. After inoculating pig carcasses with 10 pathogens (6 viruses [FMDV, ASFV, CSFV, PCV2, PRRSV, PEDV] and 4 bacteria [Lawsonia intracellularis, Clostridium perfringens type C, E. coli, Salmonella Typhimurium]) It was treated at 90℃ for 5 hours in a potassium hydroxide (KOH) liquid solution corresponding to 15% of the body weight. This method liquefies all cadaveric components and inactivates all inoculated pathogens. Based on these results, it was possible to prove that chemical treatment of pig carcasses is effective in killing pathogens and is a safe method without the risk of disease transmission. Although there are problems to be solved in the processing and operation of the chemical treatment products of livestock carcasses, the chemical treatment method of livestock carcasses can be suggested as an alternative to the current domestic burial-centered livestock carcass treatment method, preventing environmental pollution, and contributing to public health.

The development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of fluoroquinolones residues in chicken muscle using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method

  • Park, Sunjin;Kim, Hyobi;Choi, Byungkook;Hong, Chung-Oui;Lee, Seon-Young;Jeon, Inhae;Lee, Su-Young;Kwak, Pilhee;Park, Sung-Won;Kim, Yong-Sang;Lee, Kwang-jick
    • Korean Journal of Veterinary Service
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    • v.42 no.4
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    • pp.289-296
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    • 2019
  • A novel rapid procedure with liquid chromatography tandem mass spectrometry (LC-MS/MS) detection has been developed by changing various conditions including sample preparation such as QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology. This work has been involved the optimization and validation of detection method for fluoroquinolones which are widespread used in livestock especially in the chicken. Five grams of homogenized chicken muscle were extracted with QuEChERS EN and acetonitrile containing 5% formic acid and cleaned with anhydrous magnesium sulfate and C18 sorbent. The separation was performed on Acquity UPLC HSS T3 (2.1 mm×100 mm, 1.8 ㎛) column. The mobile phase A and B were composed of water containing 0.1% formic acid and acetonitrile containing 0.1% formic acid, respectively. Flow rate was 0.25 mL/min and column temperate was 40℃. LC-MS/MS with multiple reaction monitoring has been optimized for ten fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, marbofloxacin, norfloxacin, ofloxacin, orbifloxacin, pefloxacin and sarafloxacin). The method developed in this study has been presented good linearity with correlation coefficient (R2) of 0.9971~0.9998. LOD and LOQ values ranged from 0.09 to 0.76 ppb and from 0.26 to 2.29 ppb, respectively. The average recoveries were from 77.46 to 111.83% at spiked levels of 10.0 and 20.0 ㎍/kg. Relative standard deviation (%) ranged 1.28~11.90% on intra-day and 3.10~8.38 % on inter-day, respectively. This analysis method was applicable to the livestock residue laboratories and was expected to be satisfactory for the residue surveillance system.

Validation of Method Determining Marmesin in Broussonetia kazinoki Extract (닥나무 추출물의 Marmesin 성분 분석법 검증)

  • Kwon, Jin Gwan;Seo, Changon;Hong, Seong Su;Seo, Dong-Wan;Oh, Joa Sub;Kim, Jin Kyu
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.11
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    • pp.1604-1609
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    • 2016
  • An HPLC analysis method was developed for standard determination of marmesin as a functional health material in Broussonetia kazinoki extract. HPLC was performed on a $C_{18}$ Kromasil column ($4.6{\times}250mm$, $5{\mu}m$) 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 analyte was detected at 330 nm. The HPLC method was validated in accordance with International Conference on Harmonization guidelines for analytical procedures with respect to specificity, precision, accuracy, and linearity. The limit of detection and quantitation were 6.2 and $18.6{\mu}g/mL$, respectively. Calibration curves showed good linearity ($r^2$>0.9999), and the precision of analysis was satisfactory (less than 0.3%). Recoveries of quantified compound ranged from 100.35 to 101.18%. This result indicates that the established HPLC method is very useful for the determination of marker compounds in B. kazinoki 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 an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Calibration of Portable Particulate Mattere-Monitoring Device using Web Query and Machine Learning

  • Loh, Byoung Gook;Choi, Gi Heung
    • Safety and Health at Work
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    • v.10 no.4
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    • pp.452-460
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    • 2019
  • Background: Monitoring and control of PM2.5 are being recognized as key to address health issues attributed to PM2.5. Availability of low-cost PM2.5 sensors made it possible to introduce a number of portable PM2.5 monitors based on light scattering to the consumer market at an affordable price. Accuracy of light scatteringe-based PM2.5 monitors significantly depends on the method of calibration. Static calibration curve is used as the most popular calibration method for low-cost PM2.5 sensors particularly because of ease of application. Drawback in this approach is, however, the lack of accuracy. Methods: This study discussed the calibration of a low-cost PM2.5-monitoring device (PMD) to improve the accuracy and reliability for practical use. The proposed method is based on construction of the PM2.5 sensor network using Message Queuing Telemetry Transport (MQTT) protocol and web query of reference measurement data available at government-authorized PM monitoring station (GAMS) in the republic of Korea. Four machine learning (ML) algorithms such as support vector machine, k-nearest neighbors, random forest, and extreme gradient boosting were used as regression models to calibrate the PMD measurements of PM2.5. Performance of each ML algorithm was evaluated using stratified K-fold cross-validation, and a linear regression model was used as a reference. Results: Based on the performance of ML algorithms used, regression of the output of the PMD to PM2.5 concentrations data available from the GAMS through web query was effective. The extreme gradient boosting algorithm showed the best performance with a mean coefficient of determination (R2) of 0.78 and standard error of 5.0 ㎍/㎥, corresponding to 8% increase in R2 and 12% decrease in root mean square error in comparison with the linear regression model. Minimum 100 hours of calibration period was found required to calibrate the PMD to its full capacity. Calibration method proposed poses a limitation on the location of the PMD being in the vicinity of the GAMS. As the number of the PMD participating in the sensor network increases, however, calibrated PMDs can be used as reference devices to nearby PMDs that require calibration, forming a calibration chain through MQTT protocol. Conclusions: Calibration of a low-cost PMD, which is based on construction of PM2.5 sensor network using MQTT protocol and web query of reference measurement data available at a GAMS, significantly improves the accuracy and reliability of a PMD, thereby making practical use of the low-cost PMD possible.