• Title/Summary/Keyword: G7 calibration

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Qualitative and Quantitative Analysis of Thirteen Marker Components in Traditional Korean Formula, Samryeongbaekchul-san using an Ultra-Performance Liquid Chromatography Equipped with Electrospray Ionization Tandem Mass Spectrometry

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.22 no.2
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    • pp.93-101
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    • 2016
  • For efficient quality control of the Samryeongbaekchul-san decoction, a powerful and accurate an ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was developed for quantitative analysis of the thirteen constituents: allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13). Separation of the compounds 1 - 13 was performed on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ with a gradient solvent system of 0.1% (v/v) formic acid aqueous-acetonitrile. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$. Calibration curves of all compounds were showed good linearity with values of the correlation coefficient ${\geq}0.9920$ within the test ranges. The values of limits of detection and quantification for all analytes were 0.04 - 4.53 ng/mL and 0.13 - 13.60 ng/mL. The result of an experiment, compounds 2, 6, 12, and 13 were not detected while compounds 1, 3 - 5, and 7 - 11 were detected with 1,570.42, 5,239.85, 299.35, 318.88, 562.27, 340.87, 12,253.69, 73.80, and $115.01{\mu}g/g$, respectively.

Determination of Polycyclic Aromatic Hydrocarbons in Smoked Food Products (훈연식품 중 polycyclic aromatic hydrocarbons 함량 분석)

  • Seo, Ilwon;Nam, Hejung;Lee, Songyoung;Lee, Kyueun;Shin, Han-Seung
    • Food Engineering Progress
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    • v.13 no.3
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    • pp.195-202
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    • 2009
  • This study was accomplished that analysis of seven polycyclic aromatic hydrocarbons (PAHs) in smoked or nonsmoked processing foods by high performance liquid chromatography (HPLC) with fluorescence detection. The calibration line was constructed with injected different levels of standard concentration. Limit of detection (LOD) and limit of quantification(LOQ) showed higher linearity ($r^{2}$=0.998) reasonably, and recovery exhibited 0.033-0.666 $\mu$g/kg, 0.108-2.217 $\mu$g/kg and 69.31-90.14%, respectively. As a result, the samples using smoked tuna as smoked materials contained seven PAHs with different range from 0.256 to 0.486 $\mu$g/kg. The benzo[a]pyrene, indicator of PAHs, was detected to below the LOQ in two samples. Concentrations of benzo[a]pyrene in three samples were below the 2 $\mu$g/kg which is the limit of regulation. Smoked tuna sauces were detected from 0.321 to 0.552 $\mu$g/kg and not detected in drying powders. PAHs of smoked meat products were ranged from 0.720 to 2.027 $\mu$g/kg and are higher than concentration of tuna smoked samples. PAHs were very low in non-smoked foods including mustard, herb, and roasted meats.

Monitoring microbiological contamination, pre-decontamination, and irradiation status of commercial dried laver (Porphyra sp.) products (시판 유통 김의 미생물 오염도, 사전 살균처리 및 전자선 조사 여부 확인)

  • Lee, Eun-Jin;Kim, Gui-Ran;Lee, Hye-Jin;Kwon, Joong-Ho
    • Korean Journal of Food Science and Technology
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    • v.49 no.1
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    • pp.20-27
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    • 2017
  • Eighteen commercial laver (Porphyra sp.) products were purchased from Korean market and were monitored for their microbial contamination, pre-decontamination, and luminescence properties. The laver samples showed considerable variation in their microbial contamination, from $10-10^7CFU/g$ of total aerobic counts, <$10-10^2CFU/g$ of coliforms in 4 dried laver samples, and <$10-10^6CFU/g$ of yeasts and molds except in 3 samples. In addition, $10^2CFU/g$ of Bacillus cereus was found in one sample. DEFT/APC analysis was suitable for demonstrating whether the samples were pre-decontaminated or not, with DEFT/APC values lower than 2.0 log for non-heated samples and 1.0-8.5 log for heatprocessed samples. In photostimulated luminescence (PSL) calibration, 15 samples irradiated at 1 kGy showed positive (irradiated) values more than 5000 PCs. Furthermore, thermoluminescence (TL) analysis by separating the marker minerals from samples revealed the potential to be employed in identifying irradiation status by determining $1^{st}$ TL glow at $125-175^{\circ}C$ and TL ratio ($TL_1/TL_2$) of all the samples.

Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
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    • v.31 no.1
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    • pp.23-30
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    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

Simultaneous Determination of Berberine, Cinnamic Acid and Glycyrrhizin in Pharmaceutical Formulations by Capillary Electrophoresis with Diode-Array Detection (모세관 전기이동법에 의한 생약제제중 베르베린, 계피산 및 글리시리진의 동시 정량)

  • Kang, Seong Ho;Chung, Wha Jin;Yoon, Hyung Jung;Chung, Doo Soo
    • Journal of the Korean Chemical Society
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    • v.41 no.2
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    • pp.98-104
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    • 1997
  • A simple, accurate and reproducible capillary electrophoresis(CE) assay has been developed for the determination of berberine, cinnamic acid, and glycyrrhizin which are used in traditional Korean medicinal preparations. Separation of these compounds was performed in 20 mM phosphate buffer(pH 7.5) and acetonitrile(75:25, v/v) using a bare fused silica capillary($57 cm{\times}75 {\mu}m$ i.d.) at 25$^{\circ}C$. With the electric field of 350 V/cm, the time needed for the separation of berberine, cinnamic acid and glycyrrhizin was within 13 min. Calibration curves were linear for 1∼100 ${\mu}g/mL$ berberine, 0.3∼100 ${\mu}g/mL$ cinnamic acid and 2.5∼100 ${\mu}g/mL$ glycyrrhizin. The ranges of relative standard deviations(n=5) for those samples were between 0.96∼2.35%. The limits of detection(S/N=3) for berberine, cinnamic acid and glycyrrhizin were 0.5, 0.1 and 2.0 ${\mu}g/mL$, respectively. The numbers of theoretical plates were 181,000(berberine), 88,000(cinnamic acid) and 169,000(glycyrrhizin), while they were 3,100∼4,800 in HPLC.

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Quantitative Analysis of Eleven Bioactive Constituents of a Traditional Herbal Medicine, Yeonggyechulgam-tang using, Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.23 no.2
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    • pp.84-91
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    • 2017
  • This study proposes a sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry method of efficiently assessing the quality of a traditional herbal medicine called Yeonggyechulgam-tang (YGCGT). The following compounds 1 - 11, namely, liquiritin apioside (1), liquiritin (2), liquiritigene (3), coumarin (4), cinnamic acid (5), cinnamaldehyde (6), glycyrrhizin (7), atractylenolide III (8), atractylenolide II (9), atractylenolide I (10), and pachymic acid (11) were separated on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $45^{\circ}C$ eluted with a gradient condition of 0.1% (v/v) formic acid in distilled water and acetonitrile. The correlation coefficient of the calibration curve of the eleven constituents was ${\geq}0.9936$. The limits of detection and quantification of the compounds 1 - 11 were 0.06 - 4.73 ng/mL and 0.17-14.20 ng/mL, respectively. Using this analytical method, the compound 11 in lyophilized YGCGT decoction extract was not detected, while the compounds 1 - 10 were detected 0.13-166.43 mg/g.

Surface-Enhanced Raman Scattering Spectroscopic Identification of Genotoxic Nucleobase Adducts (표면강화 라만분광학을 이용한 nucleobase 유도체 분석)

  • Kim, Jae-Ho
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.313-319
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    • 1995
  • Surface-enhanced Raman scattering(SERS) spectroscopy was employed to analyze the genotoxic nucleobase adducts of benzo[a]pyrene(BP) formed through one-electron oxidation pathway. SERS spectroscopy provided sufficient resolution to distinguish if BP intermediate was bound to different nucleobases(e. g. adenine or guanine). Furthermore, SERS specroscopy was also able to detect the difference in the binding position of the adduct to the various sites of the nucleobase. The linearity of the calibration curve for N7Ade-BP ranged from 20 picogram to 800 nanogram per microliter and the detection limit under the current conditions was determined 20 picogram per microliter in a solution volume of 20 microliter.

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Analysis of Multi-class Mycotoxins and Risk Assessment in Edible and Medicinal Plants by LC-MS/MS (질량분석기를 이용한 약령시장 내 유통 식물성 식품원료의 곰팡이독소 분석 및 위해성 평가)

  • Choi, Eun jung;Ko, Suk kyung;Jo, Sung ae;Park, Young ae;Jung, Sam ju;Hong, Sung cho;Cho, Seok ju;Jung, Ji hyun;Park, Ju sung
    • Korean Journal of Pharmacognosy
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    • v.53 no.3
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    • pp.162-169
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    • 2022
  • This study investigated the mycotoxins (aflatoxin B1, B2, G1, G2, fumonisin B1, B2, ochratoxin A and zearalenone) contained in edible and medicinal plants in Seoul Yangnyeong market during 2020-2021. We analyzed contamination of mycotoxins using LC-MS/MS and evaluated risk assessment. The method was validated by assessing matrix effects, linearity, limit of detection (LOD), limit of quantification(LOQ) and recovery. Matrix-matched standard calibration was used for calibration curves showed good linearity (r2>0.999). The LOD, LOQ and recovery were 0.01-0.23 ㎍/kg, 0.04-0.71 ㎍/kg and 75.5-117.9% respectively. Mycotoxins were detected in 22 of 171 samples; aflatoxin B1 (6.66 ㎍/kg), fumonisin (7.54-64.68 ㎍/kg), ochratoxin A (4.21-10.56 ㎍/kg) and zearalenone (7.31-60.76 ㎍/kg). In the risk assessment, the MOE (Margine of Exposure) of aflatoxin B1 and ochratoxin A were in the range of 1.48×103-2.36×105. No items exceeded 100% in %TDI (Tolerable Daily Intake) of fumonisin (B1+B2) and zearalenone.

Application of Polyurethane Foam Loaded with a Schiff Base Ligand for Determination of Trace Amounts of Copper in Water Samples by Flame Atomic Absorption Spectroscopy

  • Moftakhar, Mahdieh Koorehpazan;Yaftian, Mohammad Reza;Nahaei, Samaneh;Zamani, Abbas Ali
    • Journal of the Korean Chemical Society
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    • v.58 no.3
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    • pp.283-288
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    • 2014
  • A column solid phase extraction procedure based on modified polyurethane foam (PUF) by a newly synthesized Schiff base ionophore, named 2,2'-{iminobis[propane-3,1-diylnitrilo(1E)prop-1-yl-1-ylidene]}diphenol, was developed for preconcentration step of trace amounts determination of copper ions in water samples by atomic absorption flame spectroscopy. The influence of parameters on the adsorption process such as sample pH, amount of modified PUF packed in the column, type and volume of stripping reagent and its flow rate were investigated and optimized. Under optimum experimental conditions, the calibration graph was linear in a relatively wide range ($0.005-210{\mu}g/ml$) with a limit of detection $0.002{\mu}g/ml$ of copper. The proposed method allows achieving to a concentration factor of >133. The capacity of a column (1.6 cm i.d.) packed by 6 g of PUF modified by 12 mg of the Schiff base was found to be $247.7({\pm}2.1){\mu}g$ of copper. It was found that the adsorption process was highly selective towards copper ions with respect to some associated metal ions. The presented procedure was successfully applied for determination of copper in some water samples.

Water-Soluble Vitamins Contents in Seafood-Based Dishes (수산물 조리 식품에 함유된 수용성 비타민 함량)

  • Kim, Naeun;Kim, Younghwa
    • The Korean Journal of Food And Nutrition
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    • v.33 no.4
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    • pp.390-398
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    • 2020
  • The purpose of this study was to determine the contents of water-soluble vitamins B1 (thiamine), B2 (riboflavin), B3 (niacin) and B12 (cyanocobalamin) in seafood-based dishes by using the high-performance liquid chromatography with the ultra violet and fluorescence detector. The vitamin B1, B2, B3 and B12 contents were analyzed in 29 seafood-based dishes. The method validation was performed on the method to determine the linearity, accuracy, limits of quantification, limits of detection and precision for vitamin B1, B2, B3 and B12. An excellent linearity range (R2=0.999~1.000) in the calibration curve for the water-soluble vitamins was observed. All analytical methods for the water-soluble vitamins showed the acceptable accuracy (89.4~119.7% recovery) and the precision (0.6~4.8% repeatability and 1.0~4.2% reproducibility). The highest content of vitamin B1 was 2.646 mg/100 g in the kkongchi-jorim, and the highest contents of vitamin B2, B3 and B12 were 0.370 mg/100 g, 10.971 mg/100 g, and 17.193 ㎍/100 g, respectively, in the kkongchi-gui. Our results provide reliable data on the contents of the water-soluble vitamins of seafood-based dishes in Korea.