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Analytical Method Validation of Quercetin in Changnyeong Onion Extract as a Functional Ingredient for Functional Health Food (건강기능식품 기능성원료로서 창녕양파추출액의 지표성분 Quercetin 분석법)

  • Jeon, Seon-Young;Jeong, Eun-Jeong;Baek, Jeong-Hwa;Cha, Yong-Jun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.4
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    • pp.565-569
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    • 2011
  • Validation of quercetin as a marker compound in the standardization of Changnyeong onion extract developed for functional health food was attempted by analytical method. The specificity was satisfied with retention time and photo diode array (PDA) spectrum by analysis of quercetin using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve as coefficient of correlation (R2R2) of 0.9986, and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.2 mg/L and 0.5 mg/L, respectively. Recovery rate test with quercetin concentration of 0.05, 0.075 and 0.1 mg/mL was revealed in the high range of 82.36~95.26%, 82.70~98.24% and 87.91~95.11%, respectively. The intra-day and inter-day precision in quercetin for Changnyeong onion extracts was 0.10~3.28% and 0.96~5.79%, respectively. Therefore, application of quercetin was validated in analytical method as a marker compound in Changnyeong onion extracts.

Analysis of Flumeqnine in Meats (식육 중 항생제 flumequine의 분석)

  • Kuk, Ju-Hee;Ko, Yong-Seok;Kim, Yong-Hoon;Yoon, Chang-Yong;Sun, Nam-Kyu;Kim, Eun-Jung;Seo, Jee-Woo;Park, Ji-Won;Kang, Kil-Jin
    • Korean Journal of Food Science and Technology
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    • v.41 no.1
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    • pp.7-10
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    • 2009
  • An analytical method for the determination of flumequine in meats was developed and validated using high-performance liquid chromatography with fluorescence detection. The samples were mixed with sodium sulfate and extracted with ethyl acetate. After clean-up, the residues were dissolved in mobile phase. The calibration curves showed high linearity (r2r2=0.9979) within the concentration range of 0.1-1.0 mg/kg. The limit of detection and limit of quantification were validated at 0.005 and 0.017 mg/kg, respectively. The recoveries in fortified meats ranged from 90.8 to 101.1%. The method was then validated in correspondence with the CODEX guidelines for flumequine residue in meats. Herein we monitored 150 samples of meats that were purchased in Korea (Seoul, Busan, Daegu, Daejeon, and Gwangju). Among the tested samples, flumequine was detected in 1 of beef and 1 of pork at levels in the range of 0.048-0.080 mg/kg. Overall, the flumequine residues in the tested samples were within the Maximun residue limit.

Determination of Trace-Level Perchlorate by IC-MS/MS and Distribution in the Han River (IC-MS/MS를 이용한 수중의 과염소산이온 분석방법 최적화 및 한강수계내 분포조사)

  • Kim, Hyun-Hee;Han, Ihn-Sup;Jeong, Gwan-Jo;Park, Hyeon;Han, Sun-Hee;Cho, Wan-Seon
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.4
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    • pp.349-356
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    • 2010
  • Ion chromatography (IC) coupled with conductivity detector (CD) is a common system for the determination of perchlorate in water samples. Although the IC method with CD has been widely used for the determination of trace level perchlorate ion in water, sensitivity decreases dramatically as the complexity of the matrices increases. Here we proposed the application of ion chromatography coupled with mass spectrometry (IC-MS/MS) to significantly improve selectivity of perchlorate. The mean recovery of the method was 104.4 ±± 5.7% and the relative standard deviation (RSD%) was 1.9 ±± 1.3%. The alculated method detection limit (MDL) was 0.0207 ±± 0.0099 μg/Lμg/L. The concentrations of perchlorate were minimum <0.1 μg/Lμg/L and maximum 18.3 μg/Lμg/L in source water (Namhan, Bukhan and Han River). Hongreung showed higher concentrations (1st1st-14.3 μg/Lμg/L, 2st2st-18.3 μg/Lμg/L) than the other places. And the concentrations of perchlorate were 0.18~0.34 μg/Lμg/L in the samples taken from the six water treatment plants and six intake stations in Seoul.

Development of HPLC-UV method for detection and quantification of seven organic acids in animal feed (사료 중 유기산 7종 동시분석법 개발 및 유통 사료의 모니터링)

  • Kim, Jin kug;Lee, Mi Jin;Lee, Ye Ji;Kim, Hye Jin;Jeong, Min Hee;Kim, Ho Jin
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.202-208
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    • 2016
  • 본 연구에서는 사료 첨가제로 이용되고 있는 유기산 7종(formic acid, malic acid, lactic acid, acetic acid, citric acid, fumaric acid, propionic acid)의 동시분석법 개발을 위한 연구를 실시하였다. 7종의 화합물은 표준물질의 Retention time과 UV spectra를 통해 구별하였고, 분석법 검증은 직선성, 민감성, 선택성, 정확성, 정밀성을 통하여 검증하였다. 그 결과로 LOD와 LOQ의 범위가 각각 43~26,755 μg/kg, 12-8,026 μg/kg으로 설정하였고, 평균 회수율이 79.3~95.2%로 우수하게 보였으며, intra-day, inter-day에 대한 전반적인 상대 표준 편차(%RSD)는 3.2% 미만으로 나타났다. 이와 같이 검증된 자료를 통해 유기산의 동시분석에 대한 직선성, 민감성, 선택성, 정확성 및 정밀성을 확인하였고, 높은 수준을 나타냄을 알 수 있었다. 이를 바탕으로 유기산이 검출되는 단미사료 46 가지를 분석에 적용하여 진행하였고, 정량과 동시분석 검출을 위한 방법은 RP-HPLC/UV 검출기를 이용하여 성공적으로 개발되었다. 따라서 본 연구결과를 바탕으로 하여 사료 중의 유기산의 분석이 신속하고 정확해졌을 뿐 아니라, 다른 종류의 사료 또한 이를 적용하여 효율적으로 이용할 수 있을 것으로 판단된다.

Development and validation of analytical methods for pyrifluquinazon residues determination on agricultural commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 pyrifluquinazon 잔류시험법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Kim, Mi-Ra;Lee, Eun-Mi;Kuk, Ju-Hee;Cho, Yoon-Jae;Chang, Moon-Ik;Kwon, Kisung;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.174-181
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    • 2013
  • Pyrifluquinazon is classified with a quinazoline insecticide that regulates food intake by controling the feeding behavior acting on the endocrine or nervous system of pests such as aphids and white fly. To keep safety on pyrifluquinazon residues in agricultural commodities a simple, accurate and rapid analytical method was developed and validated using high performance liquid chromatograph (HPLC-UVD). The pyrifluquinazon residues acidified with 1% formic acid in samples were extracted with acetonitrile and partitioned with hexane subsequently to dichloromethane then purified with silica solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-UVD. The method was validated using apple and pear spiked with pyrifluquinazon at 0.02, 0.05 and 0.1 mg/kg and hulled rice, pepper, soybean at 0.05 and 0.1 mg/kg. Average recoveries were 70.5~107.9% with relative standard deviation less than 10%. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional FDA and Daejeon regional FDA was followed with Codex guideline (CODEX CAC/GL 40). This method is appropriated at pyrifluquinazon residues determination and will be used as official method of analysis.

Development of Disposable Immunosensors for Rapid Determination of Sildenafil and Vardenafil in Functional Foods

  • Vijayaraj, Kathiresan;Lee, Jun Hyuck;Kim, Hyung Sik;Chang, Seung-Cheol
    • Journal of Food Hygiene and Safety
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    • v.32 no.2
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    • pp.83-88
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    • 2017
  • We introduced disposable amperometric immunosensors for the detection of Sildenafil and Vardenafil (SDF/VDF) based on screen printed carbon electrodes. The developed immunosensors were used as a non-competitive sandwich-type enzyme immunoassay with a horseradish peroxidase label. The sensors were constructed on screen printed carbon electrodes by the simple electrochemical deposition of a reduced graphene oxide and chitosan (ErGO-CS) composite. To evaluate the sensing chemistry and optimize the sensor characteristics, a series of electrochemical experiments were carried out including electrochemical impedance spectroscopy, cyclic voltammetry and amperometry. The sensors showed a linear response to SDF/VDF concentrations in a range from 100 pg/mL to 300 ng/mL. The lower detection limit was calculated to be 55 pg/mL, the sensitivity was calculated to be 1.02μAng/mL/cm21.02μAng/mL/cm2, and the sensor performance exhibited good reproducibility with a relative standard deviation (RSD) of 7.1%. The proposed sensing chemistry strategy and the sensor format can be used as a simple, cost-effective, and feasible method for the in-field analysis of SDF/VDF in functional or health supplement food samples.

Development of a Hydrogen Peroxide Sensor Based on Palladium and Copper Electroplated Laser Induced Graphene Electrode (PdCu를 전기 도금한 레이저 유도 그래핀 전극 기반의 과산화수소 측정 센서 개발)

  • Park, Daehan;Han, Ji-Hoon;Kim, Taeheon;Pak, Jungho
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.67 no.12
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    • pp.1626-1632
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    • 2018
  • In this paper, we describe the fabrication and characterization of a hydrogen peroxide (H2O2H2O2) sensor based on palladium and copper (PdCu) electroplated laser induced graphene (LIG) electrodes. CO2CO2 laser was used to form LIG electrodes on a PI film. This fabrication method allows simple control of the LIG electrode size and shape. The PdCu was electrochemically deposited on the LIG electrodes to improve the electrocatalytic reaction with H2O2H2O2. The electrochemical performance of this sensor was evaluated in terms of selectivity, sensitivity, and linearity. The physical characterization of this sensor was conducted using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), which confirmed that PdCu was formed on the laser induced graphene electrode. In order to increase the sensor sensitivity, the Pd:Cu ratio of the electroplated PdCu was varied to five different values and the condition of highest amperometric current at an identical of H2O2H2O2 concentration was chosen among them. The resulting amperometric current was highest when the ratio of Pd:Cu was 7:3 and this Pd;Cu ratio was employed in the sensor fabrication. The fabricated PdCu/LIG electrode based H2O2H2O2 sensor exhibited a sensitivity of 139.4μA/mMcm2139.4μA/mMcm2, a broad linear range between 0 mM and 16 mM of H2O2H2O2 concentrations at applied potential of -0.15 V, and high reproducibility (RSD = 2.6%). The selectivity of the fabricated sensors was also evaluated by applying ascorbic acid, glucose, and lactose separately onto the sensor in order to see if the sensor ourput is affected by one of them and the sensor output was not affected. In conclusion, the proposed PdCu/LIG electrode based H2O2H2O2 sensor seems to be suitable H2O2H2O2 sensor in various applications.

Development and Validation of Analytical Method for Decursin in Aerial Parts of Angelica gigas Nakai Extract (참당귀 지상부 추출물의 지표성분 decursin의 분석법 개발 및 검증)

  • Kim, Hee-Yeon;Lee, Ki-Yeon;Kim, Tae-Hee;Park, A-Reum;Noh, Hee-Sun;Kim, Si-Chang;Ahn, Mun-Seob
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.52-57
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    • 2019
  • Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column (3×150mm3×150mm, 3μm3μm) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation (R2R2) of 0.9994 and the limit of detection and limit of quantitation were 0.011μg/mL0.011μg/mL and 0.033μg/mL0.033μg/mL, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and 10μg/mL10μg/mL were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.

Detection of phenobarbital adulteration in dietary supplements: simultaneous analysis of 16 sedative-hypnotics and sleep-inducers by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS)

  • Lee, Ji Hyun;Choi, Ji Yeon;Park, Hanna;Min, Ah Young;Kim, Nam Sook;Park, Seong Soo;Park, Sung-Kwan;Kang, Ho-il
    • Analytical Science and Technology
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    • v.32 no.1
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    • pp.24-34
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    • 2019
  • The safety of food is occasionally questionable, as there have been some reports of products contaminated with illegal adulterants. In this study, the presence of 16 sedative-hypnotics and sleep inducers in dietary supplements was determined by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS). The UPLC method was validated, providing a linearity (R2) of more than 0.999, and LODs and LOQs that ranged from 0.2 to 0.5 and 0.6 to 1.5μgmL11.5μgmL1, respectively. The repeatabilities were 0.2-8.4 % (intra-day) and 0.3-4.5 % (inter-day), and the accuracies were 89.0-117.0 % (intra-day) and 87.8-111.9 % (inter-day). The mean recoveries of the spiked samples ranged from 98.7 to 107.3 %. The relative standard deviation (%RSD) of the stability was less than 2.4 %. Using the developed method, one sedative-hypnotic compound, phenobarbital, was detected in one of the nineteen samples tested. In addition, the major characteristic fragment ions of each target compound were confirmed using Q-Orbitrap-MS for higher accuracy. Monitoring the presence of these 16 sedative-hypnotics and sleep inducers in dietary supplements should be pursued in the interest of human health, and the results of this study confirmed that the developed method has value for this application.

Validation of analytical method and antioxidant properties of Eriobotrya japonica Lindl. Leaf extract according to extraction solvent (추출용매 조건에 따른 비파 잎 추출물의 항산화 활성 및 유효성분의 분석법 밸리데이션)

  • Kim, Hyun-Hee;Heo, Mi-Ra;Lee, Songmi;Yim, Soon-Ho
    • Korean Journal of Food Science and Technology
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    • v.51 no.4
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    • pp.301-308
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    • 2019
  • The antioxidant properties of Eriobotrya japonica leaf extract were investigated using DPPH and ABTS radical scavenging assay. The 80% ethanol extract of leaves (IC50IC50 values for DPPH and ABTS were 13.9 and 10.9μg/mL10.9μg/mL, respectively) and young leaves (IC50IC50 values for DPPH and ABTS were 20.7 and 17.3μg/mL17.3μg/mL, respectively) showed high radical scavenging activity. Additionally, the quantitative method for estimation of ellagic acid and chlorogenic acid from E. japonica leaves was optimized by HPLC/DAD. This method showed high linearity of the calibration curve with a coefficient of correlation (R2R2) equal to 0.999. The LOD values for ellagic acid and chlorogenic acid were 2.35 and 0.73μg/mL0.73μg/mL, respectively, whereas LOQ values were 7.13 and 2.22μg/mL2.22μg/mL, respectively. Recovery of the two compounds was 99.7-108.0% with RSD values less than 5.31%. These results suggest that 80% ethanol extract of E. japonica leaves could serve as a potential source of natural antioxidant for us in various industrial applications.