• Title/Summary/Keyword: liquid limits

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HPLC/DAD Method Validation of 6-Hydroxyluteolin 7-O-Glucoside Analysis from Salvia plebeia (곰보배추에 함유된 6-Hydroxyluteolin 7-O-Glucoside 분석을 위한 HPLC/DAD 분석법 밸리데이션)

  • Lee, Hak-Dong;Paje, Leo Adrianne;Choi, Jungwon;Kim, Juree;Yu, A Ram;Bae, Min-Jung;Lee, Sanghyun
    • Korean Journal of Pharmacognosy
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    • v.52 no.3
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    • pp.186-191
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    • 2021
  • We developed a method to identify and quantify 6-hydroxyluteolin 7-O-glucoside in the powder of Salvia plebeia (PS) using high-performance liquid chromatography coupled with diode array detector (HPLC/DAD) and equipped with reverse-phase INNO C18 column. The analytical method was optimized and validated using novel parameters. The obtained values for the limits of detection and quantification were 3.60 and 10.90 ㎍/mL, respectively. Calibration curve showed good linearity in the concentration range tested (0.00625-0.1 mg/mL, r2 = 1.0000), high accuracy (96.2-101.4%), and precision values (RSD ≤ 0.27%). Our analysis support the use of our method for accurately identifying and quantifying 6-hydroxyluteolin 7-O-glucoside from PS in routine analyses and large-scale extraction processes for content determination.

Recent Advances in Covalent Triazine Framework based Separation Membranes (공유결합 트리아진 구조체 기반 분리막의 최근 발전)

  • Kim, Esther;Patel, Rajkumar
    • Membrane Journal
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    • v.31 no.3
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    • pp.184-199
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    • 2021
  • As a branch of covalent organic frameworks (COF), covalent triazine frameworks (CTF) are inherently porous structures composed of networks of repeating hexagonal triazine rings fabricated via the ionothermal trimerization reaction. They also contain plenty of nitrogen functional groups that increase affinity for some chemicals while rejecting others. Because of their tunable properties, many researchers have synthesized and tested CTFs for gas and liquid separation processes. Various studies of novel CTFs, mixed CTF composites, and CTF membranes have experimented for gas adsorption/separation (e.g., CO2, C2H2, H2, etc.) and desalination. Some CTF studies have determined the limits and potentials through advanced computer simulations while subsequent experiments have tested CTFs for photocatalytic properties, suggesting recyclability for greater sustainability. In this review, the covalent triazine framework-based separation membrane is discussed.

A Study on Cover Material of Waste Landfill with Engineered Stone Sludge (폐기물 매립지의 복토재로 엔지니어드스톤 슬러지의 활용에 관한 연구)

  • Kim, Youngtae;Ahn, Kwangkuk;Kang, Hongsig
    • Journal of the Korean GEO-environmental Society
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    • v.23 no.7
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    • pp.5-10
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    • 2022
  • The industrial waste is becoming a big problem in the aspect of spatial and environmental in domestic and international. Therefore, the waste reduction and recycling policy has been being implemented as a way to solve this problem. The engineered stone sludge, which is waste, is generated duing the engineered stone production process. since engineered stone sludge is mostly treated by landfill, an increase in the amount of the sludge leads to an increase in landfill sites and treatment costs. therefore, there is a need for a method of resourcization with engineered stone sludge. So, laboratory tests (Plastic and liquid limits, compaction, unconfined compression and permeability test) were conducted to confirm the possibility of using engineered stone sludge mixed with weathered granite soil as a cover material for landfill in this study. The result shows that the mixed soil material with less that 62.5% of engineered stone sludge can be used as a cover material for landfill.

Prediction of Various Properties of Soft Ground Soils using Artificial Neural Network (인공신경망을 이용한 연약지반의 지반설계정수 예측)

  • Kim, Young Su;Jeong, Woo Seob;Jeonge, Hwan Chul;Im, An Sik
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.26 no.2C
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    • pp.81-88
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    • 2006
  • This study performed field and laboratory tests for poor subsoils taken in six regions of the country and determined undrain shear strength. Su values and preconsolidation pressure are predicted using Back Propagation neural network (BPNN) and the application of BPNN is verified. The result of BPNN shows that correlation coefficient between test and neural network result is over 0.9, which means high correlativity. Especially the neural network uses only 6 parameters such as natural water content, void ratio, specific gravity, rate of passing 200th sieve, liquid limits and plasticity index among various affecting factors to estimate value and the correlation coefficent is 0.93. The conclusions obtained in this paper are from the tests performed for poor subsoils taken in the several regions of the country. If there were more test results, the prediction and influence of various soil properties could be effectively performed by neural network.

Simultaneous Determination of Eight Sugar Alcohols in Foodstuffs by High Performance Liquid Chromatography (HPLC를 이용한 식품 중 당알코올 8종 동시분석)

  • Lim, Ho-Soo;Park, Sung-Kwan;Kwak, In-Shin;Kim, Hyung-Il;Sung, Jun-Hyun;Choi, Jung-Yoon;Kim, So-Hee
    • Journal of Food Hygiene and Safety
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    • v.26 no.1
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    • pp.16-24
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    • 2011
  • A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

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.

Determination of Aflatoxins in Nuts, Their Products and Dried Fruits Using Rapid Resolution Liquid Chromatography Coupled with Tandem Mass Spectrometry (RRLC-MS/MS를 이용한 견과류 및 그 가공품과 건조과실류의 아플라톡신 분석)

  • Choi, Su-Jeong;Park, Ju-Sung;Jung, So-Young;Son, Yeo-Joon;Lyi, Yun-Jeong;Kim, Mi-Sun;Park, So-Hyun;Lee, Sang-Me;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.43 no.6
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    • pp.702-710
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    • 2011
  • The occurrence of aflatoxins $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits was investigated. Samples were collected from local markets in Seoul and analyzed by rapid resolution liquid chromatography coupled with tandem mass spectrometry using an immunoaffinity column. The chromatography method was validated for assay of aflatoxins using linearity, accuracy, precision and limit of detection and quantification. The linearity in the concentration ranged from 0.10 to $20{\mu}g/kg$ with $R^2$ > 0.9999. Sample recoveries ranged from 71.1 to 97.2% with relative standard deviations below 4.5% for spiking levels from 1 to $10{\mu}g/kg$. The limits of detection ranged between 0.02 and $0.05{\mu}g/kg$ and the limits of quantification ranged between 0.05 and $0.10{\mu}g/kg$. The levels of aflatoxin $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits were $B_1$ 0.10 to $9.94{\mu}g/kg$, $B_2$ 0.08 to $1.54{\mu}g/kg$, $G_1$ 0.04 to $3.21{\mu}g/kg$ and $G_2$ 0.06 to $0.14{\mu}g/kg$.

Evaluation of 226Ra analysis methods using a gamma-ray spectrometer and a liquid scintillation counter (감마선분광분석기와 액체섬광계수기를 이용한 226Ra 분석법 비교 연구)

  • Ju, Byoung Kyu;Kim, Moon Su;Kim, Hyun Koo;Kim, Dong Su;Cho, Sung Jin;Yang, Jae Ha;Park, Sun Hwa;Kim, Hyoung Seop;Kwon, Oh Sang;Kim, Tae Seung
    • Analytical Science and Technology
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    • v.28 no.3
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    • pp.228-235
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    • 2015
  • The efficiency and applicability of the solid phase extraction disk method in a 226Ra analysis were examined by the gamma ray spectrometer (GRS) method using a Marinelli beaker and the liquid scintillation counter (LSC) method for groundwater. The recovered 226Ra, which was filtered by the solid phase extraction disk, was analyzed using gamma ray spectrometer The disks, which were pretreated for caulking the daughter nuclide, were sealed with polyethylene film. Distilled water was used for the blank value of the 226Ra activity. The recovery values of 214Bi and 214Pb in the solid phase extraction disk, which used 226Ra standard material, were 80% (295.21 Kev) and 104% (351.92 Kev), respectively, which were higher than 75% determined by the LSC. The injection of nitrogen gas into the measuring chamber reduced the interference values by about 10%. The detection limits of the 226Ra activity in a blank sample of 5 L were 0.17~0.40 pCi/L after 80,000 seconds of measuring time. The relationship of the 226Ra activity in the solid phase extraction disk method and in the LSC method in seven groundwater samples showed a correlation coefficient value 0.987, which implies the applicability of the solid phase extraction disk method. The results showed that 226Ra activity in groundwater using the solid phase extraction disk method has the following benefits: simple pretreatment, time saving, high recovery values, a low detection limit, and so on. Compared with the LSC method and the GRS method using the Marinelli beaker for the 226Ra analysis, the solid phase extraction disk method could be useful in groundwater samples with low levels of activities of radionuclides because the method is not restricted by the volume of the sample.

Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.161-170
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    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

A Monitoring of Aflatoxins in Commercial Herbs for Food and Medicine (식·약공용 농산물의 아플라톡신 오염 실태 조사)

  • Kim, Sung-dan;Kim, Ae-kyung;Lee, Hyun-kyung;Lee, Sae-ram;Lee, Hee-jin;Ryu, Hoe-jin;Lee, Jung-mi;Yu, In-sil;Jung, Kweon
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.267-274
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    • 2017
  • This paper deals with the natural occurrence of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in commercial herbs for food and medicine. To monitor aflatoxins in commercial herbs for food and medicine not included in the specifications of Food Code, a total of 62 samples of 6 different herbs (Bombycis Corpus, Glycyrrhizae Radix et Rhizoma, Menthae Herba, Nelumbinis Semen, Polygalae Radix, Zizyphi Semen) were collected from Yangnyeong market in Seoul, Korea. The samples were treated by the immunoaffinity column clean-up method and quantified by high performance liquid chromatography (HPLC) with on-line post column photochemical derivatization (PHRED) and fluorescence detection (FLD). The analytical method for aflatoxins was validated by accuracy, precision and detection limits. The method showed recovery values in the 86.9~114.0% range and the values of percent coefficient of variaton (CV%) in the 0.9~9.8% range. The limits of detection (LOD) and quantitation (LOQ) in herb were ranged from 0.020 to $0.363{\mu}g/kg$ and from 0.059 to $1.101{\mu}g/kg$, respectively. Of 62 samples analyzed, 6 semens (the original form of 2 Nelumbinis Semen and 2 Zizyphi Semen, the powder of 1 Nelumbinis Semen and 1 Zizyphi Semen) were aflatoxin positive. Aflatoxins $B_1$ or $B_2$ were detected in all positive samples, and the presence of aflatoxins $G_1$ and $G_2$ were not detected. The amount of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in the powder and original form of Nelumbinis Semen and Zizyphi Semen were observed around $ND{\sim}21.8{\mu}g/kg$, which is not regulated presently in Korea. The 56 samples presented levels below the limits of detection and quantitation.