• Title/Summary/Keyword: Limit of Detection

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Isolation and HPLC-DAD validation of xanthoangelol in Lespedeza bicolor extract (싸리나무 추출물의 Xanthoangelol 분리 및 HPLC-DAD 밸리데이션)

  • Woo, Hyun Sim;Kim, Yeong-Su;Oh, Yu Jin;Cho, Hae Jin;Song, Se-Kyu;Kim, Dae Wook
    • Korean Journal of Food Science and Technology
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    • v.52 no.1
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    • pp.26-30
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    • 2020
  • This study was undertaken to determine the characteristics of xanthoangelol, the major chalcone constituent derived from the extracts of different parts of Lespedeza bicolor. Xanthoangelol was isolated from the root extract using column chromatography and used as a standard for quantitative analysis. The structure of the isolated compound was established based on spectroscopic evidence. The HPLC-DAD method was validated for specificity, linearity, precision, accuracy, limit of detection, and limit of quantitation. The calibration curve of xanthoangelol had significant linearity (R2>0.9999). Limit of detection and limit of quantitation 0.018 and 0.059 ㎍/mL, respectively. The relative standard deviation values of precision test, and intra- and inter-day tests were less than 0.22 and 0.40%, respectively. In the recovery test, the accuracy ranged from 98.98-102.78% with RSD values less than 0.13%. The method validation parameters indicate the applicability of the HPLC method for quality control of food or drug formulations containing L. bicolor.

Comparison of ACFAS method and DNPH-LC method for quantitative analysis of formaldehyde in Drinking water (자동연속흐름-흡광광도법과 DNPH-LC법에 의한 먹는물 중 포름알데히드 정량분석 비교)

  • Yi, Geon-Ho;Yun, In-Chul;Kim, Yeong-Kwan;Kim, Chong-Chaul;Choi, Geum-Jong;Lee, Teak-Soo
    • Journal of Korean Society of Water and Wastewater
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    • v.27 no.6
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    • pp.827-836
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    • 2013
  • Due to the stringent drinking water quality, formaldehyde will be included in Korean drinking water standard from year 2014. However, its standard analytical method has not yet been established. This study compares two analytical methods, DNPH-LC and ACFAS with respect to their analysis principles, Method Detection Limit (MDL), Limit Of Quantitation(LOQ), precision, accuracy, reproducibility, convenience, number of samples analyzed per hour and analysis cost. These methods measure absorption intensity at 360 nm by using HPLC after DNPH-derivatization (DNPH-LC) and at 410 nm by using Automated Continuous Flow Absorption Spectrophotometer (ACFAS), respectively. Reproducibility was tested by repeating the analysis 7 times using a standard solution for each method. For DNPH-LC method, MDL was $0.5{\mu}g/L$, LOQ was $1.58{\mu}g/L$ with standard deviation of $0.16{\mu}g/L$. For ACFAS method, they were $0.27{\mu}g/L$, $0.85{\mu}g/L$L with standard deviation of $0.09{\mu}g/L$, respectively. Both methods satisfied the requirement set by the Korean drinking water quality standard. Complexity of sample pretreatment procedure for DNPH-LC method may cause large error and, consequently, the analytical result will depend on the level of skill of analyst. In contrast, ACFAS method which used only one reagent equipped with an automated injection device showed little analytical error. It costs about $5.00 and $1.00 for one sample to analyze by the DNPH-LC method and the ACFAS method, respectively. Compared to the DNPH-LC method, ACFAS method provided more reliable analytical results. In terms of convenience, easiness and analytical cost, ACFAS method was demonstrated to be superior to the DNPH-LC method. The results of this study suggested that the ACFAS method could be adapted as a proper method for determining formaldehyde content in drinking water.

Risk assessment of pesticide residues in fruits collected in Gyeonggi-do, Korea from 2006 to 2010 (경기도내 유통 과실류의 잔류농약 위해평가(2006~2010))

  • Do, Young-Sook;Kim, Jung-Beom;Kang, Suk-Ho;Kim, Nan-Young;Um, Mi-Na;Park, Yong-Bae;Oh, Mun-Seok;Yoon, Mi-Hye
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.85-97
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    • 2012
  • The monitoring of pesticide residues was performed on 33 fruit commodities collected in Gyeonggi-do, Korea from 2006 to 2010. Pesticide residues were detected in 431 samples (16.8%) of total 2,558 samples and violated in 12 samples (0.5%). Annual detection rate showed 6.9%~19.4% with the rate of violation of 0.3%~0.9%. Twenty three samples (69.7%) of 33 commodities were detected and 4 samples (12.1%) were violated. Eight pesticides (EPN, dicofol, carbaryl, procymidone, methidathion, prothiofos, fenitrothion and phenthoate) were violated and 62 pesticides were detected. Chloropyrifos was detected most frequently. The rate of detection and violation of citrus fruits in fruits showed the highest level. Organophosphorus pesticides (35%) and insecticide (57%) were detected most frequently. The hazard index (%ADI) of chronic dietary risk assessment by deterministic approach showed that the lower limit value and upper limit value for the whole population were 0.0000~0.7526 and 0.0000~1.3237 respectively. For the only consumer group, the lower limit value and upper limit value were 0.0006~9.7801 and 0.0058~15.9258 respectively. Therefore the hazard index for the whole population and the only consumer group were evaluated as a safe level.

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.

Analytical method validation of oxiracetam using HPLC (HPLC를 이용한 의약품 주성분인 옥시라세탐의 Analytical Method Validation)

  • Kim, Yoo-Gon;Seo, Houng-Seok;Won, Chan-Hee
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.587-594
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    • 2010
  • This study aims to determine that the test of medicines containing oxiracetam as their main ingredient was properly performed according to protocol. Furthermore, the study is to provide the written form of protocol in order to examine the validity of the HPLC analytical method for the quantitative analysis of oxiracetam in the finished products. In this experiment, system suitability, precision, linearity, range, accuracy, specificity, quantitative limit, and detection limit of the analytical method which was used to determine the contained quality of oxiracetam, were examined. The result shows that system suitability indicates 0.127% RSD, plate number 15081, tailing factor 0.49, and resolution 32.41. The experiment of precision reveals the result of below 0.359% for repetitiveness and among the subjects. In the linearity experiment, a coefficient of correlation ($R^2$) indicates that it is 1. The accuracy experiment satisfies the standards of the recovery test, which is minimum 98.4% and maximum 99.6%. Detection limit is 0.1 mg/L and quantitative limit was found to be 0.5 mg/L. The experiment to check the specificity also satisfies the standards, so the finished product using oxiracetam as the main ingredient is verified as suitable.

Validation of ICP-MS method for trace level analysis of Pb in plasma (혈장 중 극미량 납 분석을 위한 ICP-MS 분석법 검증)

  • Lee, Sung-Bae;Kim, Yong-Soon;Lee, Yong-Hoon;Ahn, Byung-Joon;Kim, Nam-Soo;Lee, Byung-Kook;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.28 no.5
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    • pp.309-316
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    • 2015
  • The analytical method of lead in plasma by ICP-MS was validated after securing environment within class 1,000 classification. We tested specificity and accuracy of within-run and between-run. According to measurement of the amount of suspended particulates in a clean room, 0.3~62 particles were detected in 0.3 µm size while 0.0~28.3 particles were observed in 0.5 µm size. Total suspended particulates met required environment with up to 90.3 particles. The MDL (Method detection limit) of the sample which has been fabricated using fetal bovine serum (FBS) blank was 1.77 ng/L, and LOQ (Limit of quantification) was 5.55 ng/L. The slope, intercept and correlation coefficient of the calibration curve were y=1.09×10−3x+4.88×10−2 and r=0.9999, which showed good correlation. The specificity, within-run and between-run accuracy satisfied the standard at more than 50 ng/L. The average lead concentration in plasma of the general people, current workers and retired workers was 55.4 ng/L, 440 ng/L, and 132 ng/L.

Analysis of E,E-farnesol and squalene in makgeolli using stir bar sorptive extraction coupled with gas chromatography-mass spectrometry (SBSE-GCMS를 이용한 막걸리 중의 E,E-farnesol과 squalene분석법)

  • Ha, Jaeho;Shim, You-Shin;Cho, Yongsun;Seo, Dongwon;Jang, Hyewon;Jang, Hyejin
    • Analytical Science and Technology
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    • v.27 no.1
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    • pp.60-65
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    • 2014
  • The aim of this study was to establish an analytical method for the determination of E,E-farnesol and squalene in makgeolli, which is a traditional type of Korean fermented rice wine. E,E-farnesol and squalene in makgeolli were extracted using stir bar sorptive extraction (SBSE) coupled with gas chromatography-mass spectrometry. SBSE was found to be an effective method for analyzing the E,E-farnesol and squalene levels in makgeolli. The linear dynamic range of the SBSE method for detecting E,E-farnesol and squalene ranged from 0.5 to 200 ng/mL with $R^2=0.9974$ for E,E-farnesol and 100 to 50000 ng/mL with $R^2=0.9982$ for squalene. The limit of detection and the limit of quantification using the SBSE method were 0.1 and 0.5 ng/mL for E,E-farnesol and 15.0 and 40.0 ng/mL for squalene, respectively. The average recoveries obtained were, quantitatively, 101-107% for E,E-farnesol and 98-103% for squalene, respectively, supporting the accuracy of the SBSE-GCMS method.

Methods for the Extraction of DNA from Water Samples for Polymerase Chain Reaction

  • Jung, Jae-Sung;Lee, Young-Jong
    • Journal of Microbiology
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    • v.35 no.4
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    • pp.354-359
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    • 1997
  • Methods for the extraction of DNA from water sample were approximated. Four different procedures of DNA extraction were carried out with pellets obtained from centrifugation of 4 liter water samples. The recovery efficiency and purity of DNA extracted by each method from different sources were compared. DNA yield varied with extraction methods, Method I, which involves enzymatic and freeze-thaw lysis steps and phenol and phenol-chloroform purification of extracted nucleic acid, showed a significantly higher yield and purity than the other methods. The use of glass beads in the DNA extraction methods improved the purity of DNA suitable for PCR. Bovine serum albumin in the PCR reaction mixture was useful in reducing inhibitory effects of contaminants. The efficiency of an extraction method was determined by the detection of the aer of Aeromonas hydrophila with PCR. The lower limit of detection of A. hydrophila from seeded tap water was 2 CFU/ml in PCR when method I was used for DNA preparation.

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Development of Quantitative Real-Time PCR Primers for Detection of Streptococcus sobrinus

  • Park, Soon-Nang;Kook, Joong-Ki
    • International Journal of Oral Biology
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    • v.41 no.3
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    • pp.149-154
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    • 2016
  • The purpose of this study was to develop Streptococcus sobrinus-specific qPCR primers based on the nucleotide sequence of the RNA polymerase ${\beta}-subunit$ gene (rpoB). The specificity of the primers was determined by conventional polymerase chain reaction (PCR) with 12 strains of S. sobrinus and 50 strains (50 species) of non-S. sobrinus bacteria. The sensitivity of the primers was determined by quantitative real-time PCR (qPCR) with serial dilutions of the purified genomic DNAs (40 ng to 4 fg) of S. sobrinus ATCC $33478^T$. The specificity data showed that the S. sobrinus-specific qPCR primers (RTSsob-F4/RTSsob-R4) detected only the genomic DNAs of S. sobrinus strains with a detection limit of up to 4 fg of S. sobrinus genomic DNA. Our results suggest that the RTSsob-F4/RTSsob-R4 primers are useful in detecting S. sobrinus with high sensitivity and specificity for epidemiological studies of dental caries..

An Enhanced Architecture of CMOS Phase Frequency Detector to Increase the Detection Range

  • Thomas, Aby;Vanathi, P.T.
    • JSTS:Journal of Semiconductor Technology and Science
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    • v.14 no.2
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    • pp.198-201
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    • 2014
  • The phase frequency detector (PFD) is one of the most important building blocks of a phase locked Loop (PLL). Due to blind-zone problem, the detection range of the PFD is low. The blind zone of a PFD directly depends upon the reset time of the PFD and the pre-charge time of the internal nodes of the PFD. Taking these two parameters into consideration, a PFD is designed to achieve a small blind zone closer to the limit imposed by process-voltage-temperature variations. In this paper an enhanced architecture is proposed for dynamic logic PFD to minimize the blind-zone problem. The techniques used are inverter sizing, transistor reordering and use of pre-charge transistors. The PFD is implemented in 180 nm technology with supply voltage of 1.8 V.