• Title/Summary/Keyword: Curve detection

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Simultaneous analysis for 2-thiothiazolidine-4-carboxilic acid and thiocarbamide using butanol extraction method (부타놀 추출법을 이용한 2-thiothiazolidine-4-carboxilic acid와 thiocarbamide의 동시정량에 관한 연구)

  • Lee, Sanghoi;Song, Jaesok;Yoon, youngshik;Kim, Chinyon;Won, Jonguk;Roh, Jaehoon
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.10 no.1
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    • pp.208-222
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    • 2000
  • This study was conducted to supplement limit of previous study, The objectives of this study were to select optimal conditions of high performance liquid chromatography(HPLC) operation for detecting urinary 2-thiothiazolicline-4-carboxylic acid(TTCA) and thiocarbamide simultaneously, and to evaluate recovery rates for various liquid-liquid extration method of these metabolites, The results are as follows : 1. The urinary TTCA and thiocarbamide were separate sharply when flow rate is $0.7m{\ell}/min$, using a series $C_8$ and $C_{18}$ column, 50 mM $KH_2PO_4$ : acetonitrile (93.5 : 6.5) and pH 3.5 as a mobile phase. The retention time was TTCA, $12.07{\pm}0.11$(mean${\pm}$SD, n=06), thiocarbamide, $7.85{\pm}0.01$ (mean${\pm}$SD, n=6), respectively. The calibration curve for TTCA and thiocarbamide was linear within the range 0.05 to $30{\mu}g/m{\ell}$. 2. By the liquid-liquid extration, butanol extration with $(NH_4)_2$ as a salting-out reagent was used as a simultaneous extration method for these metabolites in acid state, and recovery rates of this method are urinary TTCA, $49.6{\pm}17.7$ (mean${\pm}$SD, n=16), thiocarbamide, $43,9{\pm}5.50$ (mean${\pm}$SD, n=16), respectively 3. The precision(pooled coefficients of variation for 4 concentration) of the urinary thiocarbamide analysis was 0.03754 by butanol liquid-liquid extraction with $(NH_4)_2$ as a salting-out reagent, and TTCA was 0.04082 by ethyl acetate liquid-liquid extration with $(NH_4)_2$ as a salting out reagent The above results show that the butanol liquid-liquid extraction with $(NH_4)_2$ as a salting-out reagent in acid state, and using a series $C_8$ and $C_{18}$ column, 50 mM $KH_2PO_4$ : acetonitrile (93.5 : 6.5) and pH 3.5 as a mobile phase are suitable for the analysis of urinary TTCA and thiocarbamide simultaneously. The detection limit of TTCA and thiocarbamide was about $0.17{\mu}g/m{\ell}$, $0.07{\mu}g/m{\ell}$.

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Simultaneous determination of preservatives in sausages using liquid chromatography with electrospray ionization tandem mass spectrometry (LC-MS/MS를 이용한 소시지 중 보존료 동시분석)

  • Koh, Ba-Ra-Da;Kim, Ji-Yeon;Jang, Mi-Sun;Seo, Doo-Ri;Jung, Bo-Ram;Shin, Ji-Hyun;Lim, Jin-Taek;Kim, Yong-Hwan;Kim, Eun-Sun
    • Korean Journal of Veterinary Service
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    • v.38 no.2
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    • pp.127-136
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    • 2015
  • A simultaneous determination method was developed for nine preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methyl-, ethyl-, isopropyl-, propyl-, isobutyl- and butyl-parabens) in sausage by liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Each parameter was established by multiple reaction monitoring in negative mode. Separation was achieved on a phenyl-hexyl ($2.5{\mu}m$, $2.1{\times}150mm$, Waters) with A-20 mM ammonium acetate containing 0.1% acetic acid in water, B-Acetonitrile as mobile phase with gradient mode at a flow rate of 0.3 mL/min. The developed method was validated for specificity, linearity, accuracy and precision in sausages samples. Linearity was over 0.998 with calibration curve of the mixed standards. The mean recoveries from sausages fortified at the level of 2.0~10.0 mg/L were in range of 98.60~109.16% with RSDs lower than 8.93%. The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.0003~0.085 mg/L and 0.01~0.257 mg/L, respectively. Intra-day precision and inter-day precision were 0.45~6.16% and 2.81~13.33%, respectively. Using presently developed determination method, 33 field sausage samples from Gwangju city in Korea were screened over nine preservatives. As a result, no preservatives were detected in all samples.

Exploring the feasibility of Salmonella Typhimurium-specific phage as a novel bio-receptor

  • Choi, In Young;Park, Do Hyeon;Chin, Brayan A.;Lee, Cheonghoon;Lee, Jinyoung;Park, Mi-Kyung
    • Journal of Animal Science and Technology
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    • v.62 no.5
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    • pp.668-681
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    • 2020
  • The purpose of this study was aimed to isolate a Salmonella Typhimurium-specific phage (KFS-ST) from washing water in a poultry processing facility and to investigate the feasibility of the KFS-ST as a novel bio-receptor for the magnetoelastic (ME) biosensor method. KFS-ST against S. Typhimurium was isolated, propagated, and purified using a CsCl-gradient ultracentrifugation. Morphological characteristics of KFS-ST were analyzed using transmission electron microscopy (TEM). Its specificity and efficiency of plating analysis were conducted against 39 foodborne pathogens. The temperature and pH stabilities of KFS-ST were investigated by the exposure of the phage to various temperatures (-70℃-70℃) and pHs (1-12) for 1 h. A one-step growth curve analysis was performed to determine the eclipse time, latent time and burst size of phage. The storage stability of KFS-ST was studied by exposing KFS-ST to various storage temperatures (-70℃, -20℃, 4℃, and 22℃) for 12 weeks. KFS-ST was isolated and purified with a high concentration of (11.47 ± 0.25) Log PFU/mL. It had an icosahedral head (56.91 ± 2.90 nm) and a non-contractile tail (225.49 ± 2.67 nm), which was classified into the family of Siphoviridae in the order of Caudovirales. KFS-ST exhibited an excellent specificity against only S. Typhimurium and S. Enteritidis, which are considered two of the most problematic Salmonella strains in the meat and poultry. However, KFS-ST did not exhibit any specificity against six other Salmonella and 27 non-Salmonella strains. KFS-ST was stable at temperature of 4℃ to 50℃ and at pH of 4 to 12. The eclipse time, latent time, and burst size of KFS-ST were determined to be 10 min, 25 min and 26 PFU/ infected cell, respectively. KFS-ST was relatively stable during the 12-week storage period at all tested temperatures. Therefore, this study demonstrated the feasibility of KFS-ST as a novel bio-receptor for the detection of S. Typhimurium and S. Enteritidis in meat and poultry products using the ME biosensor method.

Feature Ranking for Detection of Neuro-degeneration and Vascular Dementia in micro-Raman spectra of Platelet (특징 순위 방법을 이용한 혈소판 라만 스펙트럼에서 퇴행성 뇌신경질환과 혈관성 인지증 분류)

  • Park, Aa-Ron;Baek, Sung-June
    • Journal of the Institute of Electronics Engineers of Korea CI
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    • v.48 no.4
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    • pp.21-26
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    • 2011
  • Feature ranking is useful to gain knowledge of data and identify relevant features. In this study, we proposed a use of feature ranking for classification of neuro-degeneration and vascular dementia in micro-Raman spectra of platelet. The entire region of the spectrum is divided into local region including several peaks, followed by Gaussian curve fitting method in the region to be modeled. Local minima select from the subregion and then remove the background based on the position by using interpolation method. After preprocessing steps, significant features were selected by feature ranking method to improve the classification accuracy and the computational complexity of classification system. PCA (principal component analysis) transform the selected features and the overall features that is used classification with the number of principal components. These were classified as MAP (maximum a posteriori) and it compared with classification result using overall features. In all experiments, the computational complexity of the classification system was remarkably reduced and the classification accuracy was partially increased. Particularly, the proposed method increased the classification accuracy in the experiment classifying the Parkinson's disease and normal with the average 1.7 %. From the result, it confirmed that proposed method could be efficiently used in the classification system of the neuro-degenerative disease and vascular dementia of platelet.

Diagnostic Value of Human Epididymis Protein 4 Compared with Mesothelin for Ovarian Cancer: a Systematic Review and Meta-analysis

  • Lin, Jia-Ying;Qin, Jin-Bao;Li, Xiao-Yan;Dong, Ping;Yin, Bing-De
    • Asian Pacific Journal of Cancer Prevention
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    • v.13 no.11
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    • pp.5427-5432
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    • 2012
  • Background and Purpose: Ovarian cancer is the leading cause of death among gynecologic cancers because of the lack of effective early detection methods. Accuracies of the human epididymis protein 4 (HE4) and mesothelin in detecting ovarian cancer have never been systematically assessed. The current systematic review aimed to tackle this issue. Methods: MEDLINE, EMBASE, and Cochrane databases were searched (September 1995-November 2011) for studies on the diagnostic performances of HE4 and mesothelin in differentiating ovarian cancer from other benign gynecologic diseases. QUADAS items were used to evaluate the qualities of the studies. Meta-DiSc software was used to handle data from the included studies and to examine heterogeneity. All included studies for diagnostic performance were combined with sensitivity, specificity, positive likelihood ratio (PLR), negative likelihood ratio (NLR), diagnostic odds ratios (DORs) with 95% confidence intervals (CIs), summary receiver operating characteristic (SROC) curves, and areas under the SROC curves (AUC). Results: A total of 18 studies and 3,865 patients were eligible for the final analysis. The pooled sensitivity estimates for HE4 (74.4%) were significantly higher than those for mesothelin (49.3%). The pooled specificity estimates for mesothelin (94.5%) were higher than those for HE4 (85.8%). The pooled DOR estimates for HE4 (26.22) were higher than those for mesothelin (24.01). The SROC curve for HE4 showed better diagnostic accuracy than that for mesothelin. The PLR and NLR of HE4 were 6.33 (95% CI: 3.58 to 11.18) and 0.27 (95% CI: 0.21 to 0.34), respectively. The PLR and NLR for mesothelin were 11.0 (95% CI: 6.21 to 19.59) and 0.51 (95% CI: 0.42 to 0.62), respectively. The combination of the two tumor markers or their combination with CA-125 increased sensitivity and specificity to different extents. Conclusion: The diagnostic accuracy of HE4 in differentiating ovarian cancer from other benign gynecologic diseases is better than that of soluble mesothelin-related protein. Combinations of two or more tumor markers show more sensitivity and specificity.

LINE-1 and Alu Methylation Patterns in Lymph Node Metastases of Head and Neck Cancers

  • Kitkumthorn, Nakarin;Keelawat, Somboon;Rattanatanyong, Prakasit;Mutirangura, Apiwat
    • Asian Pacific Journal of Cancer Prevention
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    • v.13 no.9
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    • pp.4469-4475
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    • 2012
  • Background: The potential use of hypomethylation of Long INterspersed Element 1 (LINE-1) and Alu elements (Alu) as a biomarker has been comprehensively assessed in several cancers, including head and neck squamous cell carcinoma (HNSCC). Failure to detect occult metastatic head and neck tumors on radical neck lymph node dissection can affect the therapeutic measures taken. Objective: The aim of this study was to investigate the LINE-1 and Alu methylation status and determine whether it can be applied for detection of occult metastatic tumors in HNSCC cases. Methods: We used the Combine Bisulfite Restriction Analysis (COBRA) technique to analyse LINE-1 and Alu methylation status. In addition to the methylation level, LINE-1 and Alu loci were classified based on the methylation statuses of two CpG dinucleotides in each allele as follows: hypermethylation ($^mC^mC$), hypomethylation ($^uC^uC$), and 2 forms of partial methylation ($^mC^uC$ and $^uC^mC$). Sixty-one lymph nodes were divided into 3 groups: 1) non-metastatic head and neck cancer (NM), 2) histologically negative for tumor cells of cases with metastatic head and neck cancer (LN), and 3) histologically positive for tumor cells (LP). Results: Alu methylation change was not significant. However, LINE-1 methylation of both LN and LP was altered, as demonstrated by the lower LINE-1 methylation levels (p<0.001), higher percentage of $^mC^uC$ (p<0.01), lower percentage of $^uC^mC$ (p<0.001) and higher percentage of $^uC^uC$ (p<0.001). Using receiver operating characteristic (ROC) curve analysis, $%^uC^mC$ and $%^mC^uC$ values revealed a high level of AUC at 0.806 and 0.716, respectively, in distinguishing LN from NM. Conclusion: The LINE-1 methylation changes in LN have the same pattern as that in LP. This epigenomic change may be due to the presence of occult metastatic tumor in LN cases.

Electrochemical Determination of Ag(I) Ion at Chemically Modified Carbon-Paste Electrode Containing 1,5,9,13-Tetrathiacyclohexadecane (1,5,9,13-Tetrathiacyclohexadecane 수식전극을 사용한 Ag(I)의 전기화학적 정량)

  • Ha, Kwang Soo;Jang, Mi-Kyeong;Seo, Moo Lyong
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.187-195
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    • 1997
  • Chemically modified electrodes(CMEs) for Ag(I) were constructed by incoporating 1,5,9,13-tetrathiacyclohexadecane([16]-ane-$S_4$) with a conventional carbon-paste mixture composed of graphite powder and nujol oil. Ag(I) ion was chemically deposited onto the surface of the modified electrode with [16]-ane-$S_4$ by immersion of the electrode in the acetate buffer solution(pH=4.5) containing $5.0{\times}10^{-4}M$ Ag(I) ion. And then the electrode deposited with Ag(I) was reduced at -0.3V vs. S.C.E. Well-defined stripping voltammetric peaks could be obtained by scanning the potential to the positive direction. The CME surface was regenerated with exposure to 0.1M $HNO_3$ solution and was reused for the determination of Ag(I) ion. When deposition/measurement/regeneration cycles were 10 times, the response could be reproduced with relative standard deviation of 6.08%. In case of differential pulse stripping voltammetry, the calibration curve for Ag(I) was linear over the range of $5.0{\times}10^{-7}{\sim}1.5{\times}10^{-6}M$. And the detection limit was $2.0{\times}10^{-7}M$. Various ions such as Cd(II), Ni(II), Pb(II), Zn(II), Mn(II), Mg(II), EDTA, and oxalate(II) did not influence the determination of Ag(I) ion, except Cu(II) ion.

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Determination of Pantothenic acid in Fortified Foods by HPLC (시판 영양강화식품중 판토텐산의 분석)

  • 최윤주;장재희;박혜경;박건상;구용의;황인경;김대병
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.33 no.2
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    • pp.381-385
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    • 2004
  • This study was conducted to develop an HPLC method for determining pantothenic acid in fortified foods which has typically been determined by microbiological assay (MBA) according to AOAC and Korean Food Code approved methods. Pantothenic acid was determined by reversed-phase ion-pair HPLC using UV absorption (200 nm) after extraction with 20 mM potassium phosphate solution by sonication. The recovery of spiked samples and detection limit (LOD) by HPLC were 83.5∼109.6% and 0.5 ppm (mg/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of pantothenic acid analyzed in all tested samples (n=13) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 91.9∼117.6%. There was not significant difference (p<0.01) between the HPLC and MBA methods and the equation of the regression curve was y=1.1428x-0.2269 (r=0.9842). This proposed HPLC method for determining pantothenic acid appears to be suitable for determining pantothenic acid concentrations above 0.25 mg/100 g in fortified foods.

Bioequivalence of Cefaclor Monohydrate 250mg Capsules Using an Improved HPLC Analytical Method (개선된 HPLC분석법을 이용한 세파클러 모노하이드레이트 250 mg 캡슐의 생물학적동등성)

  • Kim, Tae-Wan;Cao, Qing-Ri;Han, Sun-Young;Song, Ok-Kyoung;Sin, Kwan-Seog;Kang, Sung-Ha;Lee, Beom-Jin
    • Korean Journal of Clinical Pharmacy
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    • v.15 no.1
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    • pp.21-26
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    • 2005
  • A bioequivalence study of CKD $Cefaclor^{(R)}$ capsule (Chong Kun Dang Pharm Co., Ltd) to $Ceclor^{(R)}$ capsule (Lilly Korea Co., Ltd.) was conducted according to the guidelines of Korea Food and Drug Administration (KFDA). Twenty four healthy male Korean volunteers received each medicine at the cefaclor dose of 250 mg in a $2{\times}2$ crossover study. There was a one-week washout period between the doses. An improved high-performance liquid chromatorgraphy (HPLC) analytical method with UV detection was used to determine plasma cefaclor concentration in human volunteers for 8 hr after oral drug administration. The area under the plasma concentration-time curve from time zero to 8 hr ($AUC_{0-8hr}$) was calculated by the linear trapezoidal rule. the $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were compiled from the plasma concentration-time data. Analysis of variance was carried out using logarithmically transformed $AUC_{0-8hr}\;and\;C_{max}$. No significant sequence effect was found for all of the bioavailability parameters indicating that the cross-over design was properly performed. The $90{\%}$ confidence intervals of the $AUC_{0-8hr}$ ratio and the $C_{max}$ ratio for CKD $Cefaclor^{(R)}$ and $Ceclor^{(R)}$ were $0.9400{\leq}{\delta}{\leq}1.0345$ and $0.8858{\leq}{\delta}{\leq}1.1021$, respectively. These values were within the acceptable bioequivalence intervals of 0.80-1.25. Thus, our study demonstrated the of CKD $cefaclor^{(R)}$ capsule was bioequivalent to $Cefaclor^{(R)}$ capsule with respect to its bioavailability.

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Validation of an analytical method of oxyresveratrol for standardization of Mulberry (Morus alba L.) branch extract as a functional ingredient (상지추출물의 기능성원료 표준화를 위한 지표성분 옥시레스베라트롤 분석법 검증)

  • Jeon, Young-Hee;Choi, Sang-Won
    • Korean Journal of Food Science and Technology
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    • v.50 no.4
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    • pp.377-382
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    • 2018
  • An HPLC method was developed to quantitate a marker, oxyresveratrol (ORT), for the standardization of mulberry branch extracts (MBE) as a functional ingredient. HPLC was performed on a $C_{18}$ column with a gradient elution using 0.05% $H_3PO_4$ and acetonitrile at a flow rate of 0.8 mL/min, and detected at 320 nm. The HPLC method was validated according to Korea Food and Drug Administration (KFDA) guideline of analytical procedures with respect to specificity, linearity, accuracy and precision. Calibration curve of ORT showed high linearity ($R^2=1$), and limits of detection and quantification were 0.3 and $1.0{\mu}g/mL$, respectively. Relative standard deviation values from intra-and inter-day precision were less than 3.52 and 4.70%, respectively. Recovery rate ranged from 97.64% to 103.69%, and ORT content in MBE was approximately 3.78%. These results suggest that the HPLC method developed for the analysis of ORT in MBE is simple, efficient, and could contribute to the quality control of MBE.