• 제목/요약/키워드: HPLC analysis methods

검색결과 485건 처리시간 0.026초

국내 유통 종이팩 포장재 중 Isopropylthioxanthone(ITX) 분석 (Analysis of ITX from Commercial Carton Packs in Korean Market)

  • 엄미옥;윤혜정;최현철;전대훈;김형일;성준현;박나영;이은준;성덕화;이영자
    • 한국식품위생안전성학회지
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    • 제22권2호
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    • pp.88-92
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    • 2007
  • 식품용 종이포장재 등에 사용될 수 있는 UV 잉크 인쇄방식에는 광개시제를 이용한 경화방식 또는 전자빔을 이용한 경화방식이 주로 사용된다. 최근 유럽에서 종이팩 포장재의 광개시제로 사용될 수 있는 Isopropylthioxanthone (ITX)에 대한 검출사례가 보고 된 바 있으나, 국내에서는 종이팩 포장재 중 ITX에 대한 모니터링연구가 전무한 상태이므로 제외국 연구동향에 신속히 대응할 수 있는 ITX 분석방법을 확립하고, 확립된 분석방법을 적용하여 국내 유통 종이팩으로 포장된 식품 중 ITX 잔류량에 관한 모니터링을 실시하였다. HPLC/FLD를 이용한 ITX의 분석방법을 확립하였으며, 이때 확립된 분석방법에 대한 상대표준편차 1.09% 이내의 재현성, 상관계수 0.9991 이상의 직선성, 검출한계 0.02 ppb 및 정량한계는 0.1 ppb였다. 또한, 확립된 분석방법을 적용하여 국내 유통 중인 우유, 주스 등 종이팩으로 포장된 제품 87종을 대상으로 ITX 잔류량을 모니터링 한 결과, 모든 식품에서 ITX는 검출되지 않았다.

Collagen으로 유발된 생쥐의 관절염에 대한 당귀사역가오수유생강탕(當歸四逆加吳茱萸生薑湯)의 효과 (Effects of Danggwisayeokgaohsuyusaenggang-tang(當歸四逆加吳茱萸生薑湯) on Collagen-induced Arthritis in Mice)

  • 김민균;오민석
    • 한방재활의학과학회지
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    • 제21권2호
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    • pp.63-85
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    • 2011
  • Objectives : This study was carried out to know the effects of Danggwisayeokgaohsuyusaenggang-tang(hereinafter referred to DST) on arthritis induced by collagen on DBA/1 OlaHsd mice. Methods : For this purpose, DST was orally administered to mouse with arthritis induced by collagen II. Cytotoxicity, high performance liquid chromatograph(HPLC) analysis, arthritis index, value of immunocyte in draining lymph node and paw joint, cytokine were measured in vivo. Results : 1. The cytotoxicity against human fibroblast cells(hFCs) was not measured in any concentration. 2. In HPLC analysis, There are high peak patterns at 8 minute(min), 12 min, 35 min, 45 min. 3. The arthritis index was decreased significantly. 4. The degree of arthritis induced damage of joint of DST group is slight compared with control group in histopathologic observation(Hematoxylin and eosin stain(H&E), Masson's trichrome(M-T) staining). 5. In total cell counts of draining lymph node(DLN) and paw joint, the cells in DLN decreased significantly on DST 200 mg/kg and the cells in paw joint decreased significantly on 200 mg/kg and 50 mg/kg. 6. In DLN, $CD4^+/CD25^+$, $CD3^+/CD69^+$, major histocompatibility complex(MHC), class-II/$CD11c^+$ cells decreased significantly on DST 200 mg/kg and 50 mg/kg $CD3^+/CD8^+$ cells decreased significantly on DST 200 200 mg/kg, $CD4^+$, $CD3^+/CD44^+$ cells decreased. 7. In paw joints, $CD4^+$, $CD11b^+/Gr-1^+$ cells decreased significantly on DST 200 mg/kg and 50 mg/kg. 8. In joints, levels of $IL-1{\beta}$, IL-6, $TNF-{\alpha}$, cyclo-oxygenase-2(COX-2), NOS-II were decreased on DST 200 mg/kg and DST 50 mg/kg. 9. In analysing of cytokine in CD3/CD28 activated spleen, IL-17 was decreased significantly, IL-4 was increased significantly $INF-{\gamma}$ was decreased on DST 200 mg/kg. 10. In analysing of cytokine in collagen activated spleen, IL-17 were decreased significantly, IL-4 was increased significantly. Conclusions : This results demonstrated that DST suppressed the inflammatory progression of collagen-induced arthritis(CIA) mice and supported further studies are required to survey continuously in looking for the effective substance and mechanism in the future.

염수초 포제법에 따른 두충의 항산화 및 항염증 활성 변화 비교연구 (Salt-water Processing-dependent Change in Anti-oxidative and Anti-inflammatory Effects of Cortex Eucommiae)

  • 고원일;이진호;하인혁;정화진;이인희;이재웅;김은지;강병구;전세환;조용규;김민정
    • 한방재활의학과학회지
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    • 제27권2호
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    • pp.29-38
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    • 2017
  • Objectives The present study aimed to investigate the change in marker compounds, anti-oxidative and anti-inflammatory effects of salt-water processed Cortex Eucommiae. Methods To evaluate the influence of processing on anti-oxidant effect of Cortex Eucommiae, changes in total phenol, total flavonoid, 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) free radical scavenging, and ferric reducing antioxidant power (FRAP) between processed and raw Cortex Eucommiae were assessed. In addition, nitrite assay was conducted to determine the influence of processing on anti-inflammatory effect of Cortex Eucommiae. Cell viability was also examined as to elucidate whether processing affects cytotoxicity of Cortex Eucommiae. Finally, high-performance liquid chromatography (HPLC) analysis was conducted to monitor changes in pinoresinol diglucoside amount of processed and raw Cortex Eucommiae. Results Salt-water processed Cortex Eucommiae showed higher total phenol and flavonoid amount, compared to raw Cortex Eucommiae. Furthermore, anti-oxidative activity of processed Cortex Eucommiae was improved as discovered in DPPH, ABTS, and FRAP assays. Anti-inflammatory effect of Cortex Eucommiae was also enhanced following salt-water processing, as evidenced in nitrite assay. HPLC analysis found that the amount of pinoresinol diglucoside, widely known as the marker compound of Cortex Eucommiae, increases through salt-water processing. All experiments were performed with non-toxic concentration of Cortex Eucommiae; processing did not affect the cytotoxicity of Cortex Eucommiae up to the currently adopted concentration. Conclusions The present results support that salt-water processing of Cortex Eucommiae is beneficial in terms of marker compound amount, anti-oxidative, and anti-inflammatory activities. Additional investigations are needed to standardize the processing method of Cortex Eucommiae.

오매(烏梅)의 다성분동시분석 및 마우스를 이용한 경구 단회투여 급성독성시험 (Simultaneous determination and acute toxicity study of Fructus mume extracts in ICR mice)

  • 이인선;한창현;이철;황방연;정상혁;이영준;전원경
    • 대한예방한의학회지
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    • 제15권1호
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    • pp.37-47
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    • 2011
  • Objectives : Previous studies have shown that Fructus mume (FM) has anti-platelet effects. The present study was performed to determine the acute oral toxicity and quality control of a crude extract of FM in ICR mice. Methods : We investigated the in vivo single dose acute toxicity of FM 95% ethanol extract. This test was orally administered once by gavage to 20 male and 20 female mice at dose levels of 0 (control group), 1250, 2500 and 5000mg/kg body weight, respectively. Mortalities, clinical findings, autopsy findings and body weight changes were monitored daily for the 14 days following the administration. HPLC analysis was performed for the simultaneous determination of ursolic acid and p-hydroxycinnamic acid in FM. Reverse-phase chromatography using a C18 column and photodiode array detection at 211 nm was used for quantification of the two maker components. The mobile phase for gradient elution consists of water and acetonitrile. Results : We observed survival rates, general toxicity, change of body weight, and autopsy. The mice did not die after single oral administration of maximum dose of FM. Autopsy of animal revealed no abnormal gross finding. Therefore, $LD_{50}$ value of FM for ICR mice was more than 5000mg/kg on oral route. The HPLC analysis showed that ursolic acid and p-hydroxycinnamic acid amounts to 9.75- and 0.12% in the extract with the retention times of 47.99- and 15.38 minutes, respectively. Conclusions : These results suggest that no toxic dose level of FM in mice is considered to be more than 5000mg/kg. Consequently, it was concluded that FM have no effect on acute toxicity and side effect in ICR mice. For the quality control of FM extract, simultaneous determination of ursolic acid and p-hydroxycinnamic acid was established.

곽향의 성분 분석 및 주요 성분들의 in silico 항당뇨 타겟 단백질 탐색 (Analysis of Chemical Constituents of Agastachis Herba and in silico Investigation on Antidiabetic Target Proteins of its Major Compounds)

  • 최종근
    • 한국산학기술학회논문지
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    • 제22권4호
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    • pp.483-492
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    • 2021
  • 곽향은 식욕부진, 메스꺼움 등의 치료에 사용될 뿐만 아니라 최근에는 항당뇨 효능도 알려졌다. 본 연구에서는 곽향의 항산화력과 주요 성분들을 조사한 다음, in-silico 방법론을 적용하여 타겟 단백질들을 예측하였다. 먼저 메탄올 추출물의 DPPH와 ABTS 라디칼 소거능의 EC50 값은 각각 78.6 ㎍/mL과 31.0 ㎍/mL이었다. 이것은 ascorbic acid의 값(9.9 ㎍/mL, 5.2 ㎍/mL)과 비교할 때 항산화력이 뛰어나다고 할 수 있다. HPLC-PDA-MS/MS를 이용하여 성분들을 정성 분석한 결과, 추출물의 주요 화합물로 rosmarinic acid, tilianin, agastachoside 그리고 acacetin을 확인하였다. 이들 성분들의 항당뇨 작용 타겟 단백질을 DIA-DB 서버를 사용하여 구조 유사도와 inverse doking 방법론을 적용하여 예측하였다. 본 가상 탐색 결과, 주요 타겟 단백질들은 PPAR-γ, DPP IV, glucokinase, α-glucosidase, SGLT2, aldose reductase, corticosteroid 11-beta-dehydrogenase로 예측되었다. 그리고 이들 단백질들 중 일부는 이미 실험적으로 검증된 타겟 단백질이었다. 따라서 in silico 검색 방법이 유효하다고 생각할 수 있다. 마지막으로 활성성분들의 최적의 추출 조건을 결정하기 위하여 여러 추출 용매들로 곽향을 추출하였다. 여러 유기 용매들 중에는 메탄올이 그리고 에탄올-물 혼합용매에서는 80% 에탄올이 가장 효과적인 추출 용매로 확인되었다.

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

  • 이건호;윤인철;김영관;김종철;최금종;이택수
    • 상하수도학회지
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    • 제27권6호
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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.

구미강활탕의 성분 분석 및 LDL 산화억제 효능 연구 (Simultaneous Determination of Gumiganghwal-tang and Its Anti-atherosclerotic Effect)

  • 김온순;서창섭;신현규
    • 대한예방한의학회지
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    • 제17권3호
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    • pp.165-176
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    • 2013
  • Objective : The purpose of this study was to establish the simultaneous analysis for six compounds in Gumiganghwal-tang (GMGHT, Jiuweiqianghuo-tang) and to investigate the anti-atherosclerotic effects of GMGHT in vitro. Methods : The column for separation of six compounds was used Luna $C_{18}$ column and maintained at $40^{\circ}C$. The mobile phase for gradient elution consisted of two solvent systems, 1.0% acetic acid in water and 1.0% acetic acid in acetonitrile. The analysis was carried out at a flow rate of 1.0 mL/min with pothodiode array (PDA) detection at 254, 280, and 320 nm. The injection volume was 10 ${\mu}L$. The antioxidant activities of GMGHT were evaluated by measuring free radical scavenging activities on 2,2'-Azinobis-3-ethyl-benzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The inhibitory effects on low-density lipoprotein (LDL) oxidation were evaluated by the formation of thiobarbituric acid relative substances (TBARS), relative electrophoretic mobility (REM), and fragmentation of apolipoprotein B (ApoB)-100. Results : Calibration curves were acquired with $r^2{\geq}0.9998$. The contents of liquiritin, ferulic acid, baicalin, baicalein, glycyrrhizin, and wogonin in GMGHT were 1.784, 1.693, 37.899, 0.258, 1.869, and 0.034 mg/g, respectively. The GMGHT showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction ($RC_{50}$) against ABTS and DPPH radicals were 72.51 ${\mu}g/mL$ and 128.49 ${\mu}g/mL$. Furthermore, GMGHT reduced the oxidation properties of LDL induced by $CuSO_4$. Conclusion : HPLC-PDA is considered as an available and convenient method for quality control and standardization of GMGH and GMGHT has potentials on anti-atherosclerosis by anti-oxidative effect and suppressive effect on LDL oxidation.

오디 재배양식 및 지역에 따른 균핵병 방제 효과와 농약 잔류 특성 (Pest Control and Analysis of Residual Pesticides of Mulberry Fruit and Leaf against Popcorn Disease by Cultivated Type and Region)

  • 김현복;이영보;임정대;이소라;구본우;권해용
    • 한국약용작물학회지
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    • 제28권6호
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    • pp.435-444
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    • 2020
  • Background: As the Positive List System (PLS) is implemented in broad application to agricultural products, attention to the correct use of pesticides is also needed in the production of mulberry leaves and fruit. In this regard, three types of pesticides against mulberry popcorn disease were applied 2 - 3 times both in the field and greenhouses to prepare safety standards. Residual pesticide analysis was conducted on mulberry fruits and leaves. Methods and results: Three pesticieds, thiophanate-methyl, thiophanate-methyl·triflumizole and fluopyram registered as PLS pesticides for mulberry popcorn disease, were sprayed in the Wanju and in Buan regions, after which residual pesticide analysis was conducted using high-performance liquid chromatography (HPLC). As three pesticieds were either undetected or below the permissible level in mulberry fruit, demonstrating that they were suitable for safe spraying. However, 5.6 mg/kg of thiophanate-methyl was detected in the greenhouse after three application, which was slightly above maximum residue limit (MRL). Furthermore the level of thiophanate-methyl·triflumizole was higher than 0.2 mg/kg ("Gwasang No. 2" variety, spraying twice) or similar to 0.09 mg/kg ("Daesim" variety, spraying thrice) the permissible level (0.1T mg/kg) as the thiophanate-methyl was detected in mulberry leaves in the greenhouse. Conclusions: The spraying frequency for controlling mulberry popcorn disease in greenhouses should be limited to two times or less, especially when mulberry leaves are treated with thiophanate-methyl·triflumizole careful consideration is required if the leaves are to be used as food materials.

비임상시험관리기준 시스템에서 고성능액체크로마토그래피 분석법 정확도 검증의 필요성 (Necessity of high-performance liquid chromatography validation in good laboratory practice systems)

  • 양수빈;김창열
    • 한국응용과학기술학회지
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    • 제41권2호
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    • pp.172-187
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    • 2024
  • 비임상시험관리기준에서 독성시험 전 분석법 밸리데이션은 농도 설정 및 시료 제조 측면에서 중요하다. 시험기관에서는 의뢰받은 시험물질 2종에 대한 밸리데이션을 고성능액체크로마토그래피를 이용하여 수행한 결과 특이성, 시스템 적합성, 직선성, 일내 재현성, 균질성, 안정성, 농도분석, 품질관리를 판정 기준에 만족하는 분석방법을 확립 및 검증하였다. 하지만 의뢰기관의 시험성적서상 표준물질 함량은 시험기관의 결과보다 1.34배, 1.17배 높은 결과로 나타나 비임상시험관리기준에 적합한 분석법 밸리데이션을 통한 결과 도출이 신뢰성과 안정성 확보 측면에서 중요함을 확인하였다.

쪽잎 추출 산가수분해 인디고의 특성 (Characteristics of Acid Hydrolysis Indigo Extracted from Indigo(Polygonum tinctorium L.) Leaves)

  • 고인희;최태호
    • 펄프종이기술
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    • 제48권3호
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    • pp.57-65
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    • 2016
  • Indigo (Polygonum tinctorium L.) is a typical blue dye which had been used from ancient times. This study was going to shade the complicated traditional methods extracting indigo dye by the fermentation and producing as adsorbate on calcium hydroxide, which says so called as the 'Indigo lime'. Accordingly we were going to make indigo through the hydrolysis of the hot water extractives of indigo leaves simply. During hot-water extraction, ${\beta}$-glucosidase which required hydrolysis of the linkage between indigo and glucose was not activated. To achieve this goal, indican was acid-hydrolyzed to glucose and indigo. The acetic acid, citric acid, hydrochloric acid, and sulfuric acid were used for the hydrolysis of hot water extractives. The hydrolysis conditions of extractives performed in water bath at $80^{\circ}C$ for 120 minutes and in an autoclave for 120 minutes. In the acid hydrolysis of extracted indican by hot water, the indican yields of acetic acid and hydrochloric acid hydrolysis were higher than sulfuric acid in water bath. Also, the indican yield of hydrochloric acid hydrolysis was better than sulfuric acid in autoclave. The hot water extracted indican was confirmed by HPLC analysis and its structure was confirmed by UV-Vis and FT-IR spectroscopy, compared with isolated indigo and commercial synthesized indigo. This improved extraction and hydrolysis methods can be replace the traditional indigo making method.