• Title/Summary/Keyword: HPLC/PDA

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The Optimization and Verification of an Analytical Method for Sodium Iron Chlorophyllin in Foods Using HPLC and LC/MS (식품 중 철클로로필린나트륨의 HPLC 및 LC/MS 최적 분석법과 타당성 검증)

  • Chong, Hee Sun;Park, Yeong Ju;Kim, Eun Gyeom;Park, Yea Lim;Kim, Jin Mi;Yamaguchi, Tokutaro;Lee, Chan;Suh, Hee-Jae
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.148-157
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    • 2019
  • An optimized analytical method for sodium iron chloriphyllin in foods was established and verified by using high performance liquid chromatography with attached diode array detection. An Inertsil ODS-2 column and methanol-water (80:20 containing 1% acetate) as a mobile phase were employed. The limit of detection and quantitation of sodium iron chloriphyllin were 0.1 and 0.3 mg/kg, respectively, and the linearity of calibration curve was excellent ($R^2=0.9999$). The accuracy and precision were 93.9~104.95% and 2.0~7.7% in both inter-day and intra-day tests. Recoveries for candy and salad dressing were ranged between 93 and 104% (relative standard deviation, (RSD) 0.3~4.3%), and between 83 and 115% (RSD 1.2~2.0%), respectively. Liquid chromatography mass spectrometry was used to verify the main components of sodium iron chlorophyllin which were Fe-isochlorin e4 and Fe-chlorin e4.

Modification and Validation of Analytical Method for Oxypaeoniflorin and Paeoniflorin in Moutan Cortex Radicis Extract (목단피 추출물의 Oxypaeoniflorin 및 Paeoniflorin의 분석법 개선 및 검증)

  • Choi, Seung-Hyun;Yoo, Chang-Kil;Hwang, Ji-Hyun;Lee, Gi-Bbeum;Lee, Young-Jin;Lee, Boo-Yong;Lee, Ok-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.9
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    • pp.1091-1096
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    • 2017
  • The aim of this study was the validation of a modified analytical method for determination of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis extract. For validation of the analytical method, we modified established analytical methods and validated improvement. For validation, the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification of oxypaeoniflorin and paeoniflorin were measured by high performance liquid chromatography. The results show that the correlation coefficients of the calibration curve for oxypaeoniflorin and paeoniflorin were 1.0000 and 0.9998, respectively. The LOD for oxypaeoniflorin and paeoniflorin were $0.23{\mu}g/mL$ and $0.25{\mu}g/mL$, respectively. The inter-day and intra-day precision values of oxypaeoniflorin and paeoniflorin were 0.70~3.19% and 1.74~2.43%, and 0.32~0.92% and 0.62~2.28%, respectively. The inter-day and intra-day accuracies of oxypaeoniflorin and paeoniflorin were 98.33~102.11% and 97.72~118.12%, and 98.44~101.56% and 97.10~112.00%, respectively. Therefore, the analytical method was validated for the detection of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis.

Method Validation for Determination of Lignan Content in Fermented Sesame by Bioconversion (생물전환된 참깨 발효물의 Lignan 화합물의 분석법 검증)

  • Jung, Tae-Dong;Kim, Jae-Min;Choi, Sun-Il;Choi, Seung-Hyun;Cho, Bong-Yeon;Lee, Jin-Ha;Lee, Sang Jong;Park, Seon Ju;Heo, In Young;Lee, Ok-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.5
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    • pp.646-652
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    • 2017
  • The aim of this study was to investigate method validation for determination of sesamol, sesamin, and sesamolin in non-fermented sesame and fermented sesame by bioconversion. For validation, the specificity, linearity, precision, accuracy, limits of detection (LOD), and quantification (LOQ) of sesamol, sesamin, and sesamolin were measured by HPLC. Linearity tests showed that the coefficients of calibration correlation ($R^2$) for sesamol, sesamin, and sesamolin were 0.9999. Recovery rates of lignan contents in non-fermented and fermented sesame were high in the ranges of 100.27~115.10% and 98.43~114.90%, respectively. The inter-day and intra-day precisions of sesamin and sesamolin analyses for non-fermented and fermented sesame were 0.27~1.94% and 0.25~0.69%, respectively. The LOD and LOQ were $0.23{\sim}0.34{\mu}g/g$ and $0.70{\sim}1.03{\mu}g/g$, respectively. These results indicate that the validated method is appropriate for the determination of sesamol, sesamin, and sesamolin.

A Survey on the Pesticide Residues and Risk Assessment for Agricultural Products on the Markets in Incheon Area from 2010 to 2012 (인천광역시 유통 농산물의 최근 3년간의 잔류농약 실태 및 안전성 조사)

  • Kim, Hye-Young;Lee, Soo-Yeon;Kim, Cheol-Gi;Choi, Eun-Jeong;Lee, Eun-Ju;Jo, Nam-Gyu;Lee, Jea-Man;Kim, Yong-Hee
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.61-69
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    • 2013
  • BACKGROUND: This survey was done to investigate the pesticide residues and to assess their risk on agricultural products on the Markets in Incheon from 2010 to 2012. METHODS AND RESULTS: The total number of samples were 16,025 for agricultural products and these were analyzed by multi-residue method using GC-ECD/NPD, GC-MS, LC-MS/MS and HPLC-PDA/FLD. The violation rates of the samples over maximum residue limits(MRLs) of pesticide residues established by Korean Food and Drug Administration in the survey of 2010, 2011 and 2012 were 1.2%, 0.8% and 0.7%, respectively. CONCLUSION(S): Of the total violated samples, more than 75% of the rates were recorded from the samples of leafy vegetables. Most commonly encountered agricultural commodities over MRLs were Chwinamul, perilla leaves and crown daisy. The pesticides detected yearly over MRLs during three years were endosulfan, chlorpyrifos, diazinon, lufenuron, chlorothalonil, flutolanil, procymidone, ethoprophos. Estimated daily intakes compared to acceptable daily intakes, except radish and Welsh onion, is estimated less harm on human in 10 kinds of pesticides which frequently occurred violation.

Analysis of Formaldehyde in Fisheries Products (수산물 중 포름알데히드 함량분석)

  • Kim, Hyun-Ah;Jang, Jin-Wook;Kim, Do-Hyeong;Lee, Hwee-Jae;Lee, Soo-Min;Chang, Ho-Won;Lee, Kwang-Soo;Lee, Chang-Hee;Jang, Young-Mi;Kang, Chan-Soon
    • Korean Journal of Food Science and Technology
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    • v.43 no.1
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    • pp.17-22
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    • 2011
  • In this study, formaldehyde in various fisheries products was previously derivatized with acetylacetone and subsequently analyzed by using HPLC-PDA. The formaldehyde contents ranged from 0.07 to 73.74 mg/kg. The compound was significantly higher in both mollusks (0.34-12.38 mg/kg) and crustaceans (0.09-73.74 mg/kg) than in fish (0.07-3.35 mg/kg) and shellfish (0.50-3.90 mg/kg). This difference was due to storage time and temperature. In general, fish and shellfish are sold live or in refrigerated form with shorter a shelf-life, but mollusks and crustaceans are distributed in cold or frozen systems with a longer shelf-life. Using food intake data from a report of the National Health and Nutrition Survey, the daily human exposure level to formaldehyde was 0.58% of the ADI. The results from this study might provide fundamental information to confirm naturally-originating or fraudulent formaldehyde treatment in fisheries products.

Monitoring of Pesticide Residues and Risk Assessment in Some Fruits on the Market in Incheon, Korea (인천지역 유통 과일 중 잔류농약 모니터링 및 위해성 평가)

  • Chung, Se Jin;Kim, Hye Young;Kim, Ji Hyeung;Yeom, Mi Suk;Cho, Joong Hee;Lee, Soo Yeon
    • Korean Journal of Environmental Agriculture
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    • v.33 no.2
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    • pp.111-120
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    • 2014
  • BACKGROUND: This study was conducted to investigate the levels of pesticide residues in fruits and to assess their risk to human health. METHODS AND RESULTS: Monitoring of 215 samples of fruits collected from local markets in incheon during 2013 was performed. 259 pesticides were analyzed by multi-residue method and Quick, Easy, Cheap, Effective, Rugged, and safe/Mass/Mass(QuEChERS/MS/MS) method using Gas Chromatography-Electron Capture Detector/Nitrogen Phosphorus Detector(GC-ECD/NPD), GC-MS, LC(Liquid Chromatography-Mass/Mass(LC-MS/MS) and High Performance Liquid Chromatography-Photodiode Array/Fluorescence Detector(HPLC-PDA/FLD). In 56.3% of the samples detected pesticide residues and were not found to exceed Maximum Residue Limits(MRL). The highest detected samples were found in citrus fruits(83.9%). Among the detected compounds, carbendazim(13.1%), imazalil (11.7%), thiabendazole(10.7%) and fludioxonil(9.8%) were frequently found in fruits. A risk assessment of pesticide residues in fruits was performed by calculating Estimated Daily Intake(EDI) and Acceptable Daily Intake(ADI). Also, we were evaluated removal efficiency of pesticide residues by washing and peeling. The removal efficiency of pesticide residues in citrus and tropical fruits by peeling processes were 91.6%. After the washing process, the removal rates were 43.1%(Cherry, Grape, Blueberry). CONCLUSION: The level of pesticide residues in fruits was within the MRL. The range of %ADI values was from 0.00011 to 0.98795%. The process of washing or peeling reduces the level of pesticide residues. The results of this research concluded that the detected pesticides are not harmful to human being.

Changes of Organic Acids and Free Fatty Acids During the Ripening of Emmental Cheese (에멘탈치즈의 숙성 중 유기산과 유리지방산의 변화)

  • Shin, Yong-Kook;Oh, Nam-Su;Nam, Myoung-Soo
    • Food Science of Animal Resources
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    • v.31 no.6
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    • pp.928-934
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    • 2011
  • The objective of this study was to characterize the lactate metabolism and lipolysis in Emmental cheese made of Korean raw milk throughout the ripening periods; 14 d at $10^{\circ}C$, 42 d at $23^{\circ}C$, and 30 d at $4^{\circ}C$. Emmental cheese was made using a commercial starter culture with propionic acid bacteria (PAB) and without PAB as a control on the pilot plant scale. Changes in the contents of five organic acids (citric, lactic, formic, acetic, and propionic acid) and individual free fatty acids (FFAs) were measured using HPLC/PDA and GC/FID. As a result of propionic fermentation by PAB, the concentration of acetic acid and propionic acid increased up to 1.5 and 6.1 g/kg, respectively and the most dramatic increased occurred when incubated in the hot room ($23^{\circ}C$). Lactic, citric, and formic acid contents were 2.6, 2.5 and 0.8 g/kg at the end of ripening, respectively. As a result of lipolysis, the amount of total FFAs was 6,628.2 mg/kg. Compared to the control, levels of individual FFAs from butyric (C6:0) to linoleic (C18:2) acids increased significantly (p<0.05) during the ripening period. Especially, 65.1% of total FFAs was released in the $23^{\circ}C$ room and the most abundant FFAs were palmitic (C16:0), stearic (C18:0) and oleic acid (C18:1). These results demonstrated that the lipolysis of Emmental cheese was strongly affected by bacterial lipase from PAB.

Simultaneous Analysis and Anti-allergic Effect of Mume Fructus (오매(烏梅)의 다성분 동시분석 및 항알러지 효과)

  • Seo, Chang-Seob;Ha, Hyekyung;Lee, Ho Young;Lee, JunKyung;Jung, Dayoung;Lee, Jin-Ah;Shin, Hyeun Kyoo
    • Korean Journal of Pharmacognosy
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    • v.43 no.4
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    • pp.279-285
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    • 2012
  • The Mume Fructus (MF) has been used for relieves cough, arrests arrest chronic diarrhea, treat fluid depletion, and treat ascariasis in Korea. In this study, a high-performance liquid chromatography (HPLC) method was established for simultaneous determination of six main components of MF. Additionally, we were investigated the anti-inflammatory and anti-allergic effects of MF extract on lipopolysaccharide (LPS)-treated RAW264.7 cells and tumor necrosis factor (TNF)-${\alpha}$/interferon (IFN)-${\gamma}$-treated HaCaT cells. The analytical column for separation was used a Gemini $C_{18}$ column maintained at $40^{\circ}C$. The mobile phase consisted of 1.0% (v/v) acetic acid in water (A) and 1.0% (v/v) acetic acid in acetonitrile (B). The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 280 nm and 320 nm. We evaluated the inhibitory effect of MF extract on the production of inflammatory markers, nitric oxide (NO) and prostaglandin $E_2$ ($PGE_2$) in LPS-stimulated RAW264.7 cells and thymus- and activation-regulated chemokine (TARC/CCL17) in TNF-${\alpha}$/IFN-${\gamma}$-treated HaCaT cells, respectively. We confirmed the genes expression related with TARC, macrophage-derived chemokine (MDC/CCL22) and regulated on activation, normal T cell expressed and secreted (RANTES/CCL5) in HaCaT keratinocyte cells by MF extract. The contents of the five compounds in MF were 0.22-1.01 mg/g. Also, the MF extract show inhibition of about 78% and 75% on NO and $PGE_2$ production at the concentration 1000 mg/mL in RAW264.7 cells. MF extract suppressed the hTARC level and genes expression such as TARC, MDC, and RANTES on TNF-${\alpha}$/IFN-${\gamma}$-treated HaCaT cells.

Dissipation characteristics of mandipropamid and thiamethoxam for establishment of pre-harvest residue limits in lettuce (상추의 생산단계 잔류허용기준 설정을 위한 농약 Mandipropamid 및 Thiamethoxam의 잔류소실특성 연구)

  • Yang, Seung-Hyun;Lee, Jae-In;Choi, Hoon
    • Journal of Applied Biological Chemistry
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    • v.63 no.3
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    • pp.267-274
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    • 2020
  • The dissipation characteristics and kinetics of fungicide mandipropamid and insecticide thiamethoxam in lettuce under greenhouse conditions were investigated at three different lettuce-growing fields for estimating the pre-harvest residue limits (PHRLs). The analytical methods were fully validated for the quantitation of pesticide residues using High-Performance Liquid Chromatography-Photo Diode Array detector or Ultraviolet-Visible Detector and applied to real samples. The lettuces suitable for shipment were harvested during 10 days including pre-harvest interval after treatment at the recommended dose by safe-use guidelines. The initial mean residues in different fields were 6.68-17.87 and 4.96-8.31 mg/kg for mandipropamid and thiamethoxam, respectively, which decreased to 16-54 and 14-44% in 10 days. The clothianidin, a metabolite of thiamethoxam, was detected in <0.02 to 0.37 mg/kg. The dissipation of both pesticides followed first-order kinetics over a period of 10 days after application. Based on the residue data, the mean dissipation rate constant (λ) and biological half-lives (T1/2) were estimated to be -0.1060 and 6.5 days of mandipropamid and -0.1236 and 5.6 days of thiamethoxam. The PHRLs for lettuce on the 10th and 5th day before harvesting were calculated to be 63.24 and 43.56 mg/kg for mandipropamid, and 44.66 and 25.88 mg/kg for thiamethoxam, with -0.0746 and -0.1091 of the upper 95% confidence intervals of dissipation rate constant, respectively. This work would be useful as guidance for adjusting the shipment date and contribute to stabilizing the income of farmers in Korea.

Determining Anti-impotence drug-like compounds in Food (식품 중 발기부전치료제 및 유사물질의 분석)

  • Choi, Dongmi;Im, Mooheg;Lee, Kyungjin;Kwon, Kwangil;Jeong, Jiyoon;Park, Gunsang;Hong, Mooki;Lee, Chulwon
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.520-526
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    • 2004
  • To determine 6 anti-impotence drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil and hongdenafil in food, simultaneously, high performance liquid chromatography was applied. In the case of solid sample, it was extracted in organic solvents after homogenizing with mortar and pestle. Whereas liquid sample was just diluted in water and then extracted in organic solvents. Maximum lengths of UV for targets have been identified on photodiode array spectra. As results, vardenafil, hongdenafil, hydroxyhomosildenafil, sildenafil, homosildenafil, and tadalafil were eluted in order using $C_{18}$ column in acetonitrile containing phosphoric acid as the mobile phase. The maximum wavelength (${\lambda}_{max}$) was 216 nm for vardenafil, 233 and 282 nm for hongdenafil, 222 and 293 nm for hydroxyhomosildenafil, sildenafil and homosildenafil, and 284 nm for tadalafil. The overall recoveries were ranged from 95% to 109% and the limit of detection was about 0.04 mg/kg at signal/noise>3. Levels of targets in the selected food samples were 1.7 (hongdenafil) ~ 63 (tadalafil) mg/one dose.