• 제목/요약/키워드: HPLC analysis methods

검색결과 481건 처리시간 0.03초

자호(紫胡) 사이코사포닌 정량분석방법(定量分析方法) 비교(比較) (Comparison of Analytical Methods for Saikosaponins in Bupleurum falcatum L.)

  • 김관수;이승택;성낙술;이정일;채영암
    • 한국약용작물학회지
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    • 제3권3호
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    • pp.226-232
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    • 1995
  • 자호(紫胡) saikosaponin정량(定量)에 대한 추출방법(抽出方法) 및 기기분석조건별(器機分析條件別) 비교분석시험(比較分析試驗)결과는 다음과 같다. 1. HPLC를 이용한 시호 사포닌 정량은 산처리하는 방법에서 무처리 방법보다 분석시간이 더 단축되었다. 2. 추출방법상 상온추출이 수율이 높으나 가온 환류추출에 의해 분석시간이 짧고 양호한 크로마토그람을 얻을 수 있었다. 3. 시호 사포닌 분석시 HPTLC법이 HPLC법보다 대량신속측면에서 양호하나 신뢰도가 떨어졌다. 4. 따라서 시호 사포닌의 추출 및 분석은 가온환류추출과 산처리하는 분석방법이 신속한 분석방법으로 적당하였으며, 성분육종을 위한 간이검정기술로서는TLC 이용 분석이 유리할 것으로 생각되었다.

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고성능액체크로마토그래피에 의한 Isothiazolinone Components의 분석에 관한 연구 (A Study on the Analysis of Isothiazolinone Components by High Performance Liquid Chromatography)

  • 김종규;이덕희
    • 한국환경보건학회지
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    • 제18권2호
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    • pp.102-105
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    • 1992
  • 냉각탑, 제지산업, 일반 산업용수 등에 사용되는 산업용 방부제의 유효 성분 isothiazolinone components 즉, 2-methyl-4-isothiazolin-3-one(unchlorinated compound)과 5-chloro-2-methy14-isothiazolin-3-one(chlorinated compound)을 고성능액체크로마토그래피로서 분리, 정량하였다. 역상의 C$_{18}$ column (15 cmX3.9 mm I.D.)을 사용하였으며 자외선 검출기의 파장 254 nm에서 methanol-0.4% acetic acid(40 : 60)의 이동상, methanol-0.4% acetic acid(30: 70)의 추출 및 주입용매 조건으로 HPLC 분리를 시도한 결과 unchlorinated compound는 10~32,400 mg/l 범위에서, 그리고 chlorinated compound는 120~107,400 mg.l의 범위에서 직선성을 보였다. 내부 표준물질로서 dimethyl phthalate를 사용하였으며, unchlorinated compound, chlorinated compound 및 내부 표준물질의 순서로 븐리가 일어났고 총 분리시간은 6.41분이었다. 상기의 조건으로 시험물질을 분석, 정량한 결과 예측농도치에 근접한 수치를 얻었다.

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HPLC-PDA를 이용한 오약순기산 중 6종 성분의 동시분석 (Simultaneous Analysis of Six Constituents in Oyaksungi-san using HPLC-PDA)

  • 서창섭;김정훈;신현규
    • 대한한의학방제학회지
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    • 제20권2호
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    • pp.37-46
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    • 2012
  • Objectives : Oyaksungi-san(Wuyaoshunqisan) has been used for treatment of stroke and rheumatoid arthritis in Korea. In this study, a simple and accurate high-performance liquid chromatography(HPLC) method was established for simultaneous determination of six main components, liquiritin, ferulic acid, naringin, hesperidin, neohesperidin, and glycyrrhizin in Oyaksungi-san, a traditional Korean herbal prescription. Methods : The analytical column for separation of six constituents was used a Gemini $C_{18}$ column maintained at $40^{\circ}C$. The mobile phase consisted of two solvent systems, 1.0% (v/v) acetic acid in $H_2O$ (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient flow. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254 nm for glycyrrhizin, 280 nm for liquiritin, naringin, hesperidin, and neohesperidin, and 320 nm for ferulic acid. Results : Calibration curves were acquired with $r^2$ values ${\geq}0.9998$. The results of recovery test were 91.58%-105.90% with a relative standard deviations (RSDs, %) value less than 2.0%. The values of RSD for intra- and inter-day precision were 0.03%-1.72% and 0.03%-1.63%, respectively. The contents of the six compounds in Oyaksungi-san were 0.33-9.30 mg/g. Conclusions : The newly established HPLC method will be helpful to improve quality control of Oyaksungi-san.

식품 중 안나토색소 분석법 최적화 연구 (Optimization of Analytical Method for Annatto Pigment in Foods)

  • 이지연;박주희;이지현;서희재;이찬
    • 한국식품위생안전성학회지
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    • 제36권4호
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    • pp.298-309
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    • 2021
  • 본 연구의 목적은 식품 중 안나토색소를 검출하기 위하여 주성분인 cis-bixin과 cis-norbixin의 동시분석법을 개발하는 것이다. 최적 시험법 확립을 위해 국내외 기관 중 유럽식품안전청, 일본 후생노동성, 우리나라 식품의약품안전평가원의 HPLC분석법들을 비교 및 검토하였다. 그리고 직선성, 검출한계, 정량한계 및 분석시간을 고려하여 최적 HPLC 동시분석조건을 선택 후 여러 식품에 적용가능한 최적 전처리법을 개발하였다. 식품의약품안전평가원 HPLC 분석법이 가장 우수한 직선성(R2≥0.999)을 보였으며, cis-norbixin 및 cis-bixin에 대한 검출한계와 정령한계가 각각 0.03과 0.05 ㎍/mL 그리고 0.097과 0.16 ㎍/mL로 낮게 나타났다. 모든 보고된 전처리방법은 여러 식품적용에 한계가 있었으며, 어육 및 육가공품, 가공치즈, 음료의 주요 세 식품군 모두에 대해서 높은 회수율을 보이는 최적 전처리법이 새롭게 확립되었다. 이 전처리 방법은 cis-norbixin과 cis-bixin에 대해서 98% 이상의 우수한 동시 회수율을 나타냈었다. 새로운 전처리방법이 적용된 분석법은 두 성분에 대해 모두 결정계수(R2) 1로서 높은 직선성을 나타냈으며, 정확도(회수율)와 정밀도(%RSD)가 각각 평균 98% 및 0.4-7.9 이었다. 이러한 결과로부터 최적화된 분석시험법은 식품 중 안나토색소의 cis-norbixin과 cis-bixin 두 성분 동시분석에 매우 적합한 것으로 판단되었다.

가미삼황산(加味三黃散) 분획물(SH-21-B)의 지표성분 정량과 구조활성상관(QSAR) 예측 (HPLC analysis of Gami-Samhwang-San and prediction of active compounds using QSAR)

  • 유영법
    • 대한암한의학회지
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    • 제11권1호
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    • pp.95-103
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    • 2006
  • Objective: Gami-Samhwang-San, a herbal prescription for obesity treatment, is composed of seven crude herbs such as Ephedrae Herba, Scutellariae Radix, Acori Gramineri Rhizoma, Polygalae Radix, Typhae Pollen, Armeniacae Semen, Nelumbo Folium. This study was aimed to evaluate marker substances in n-butanol fraction (SH-21-B) from Gami-Samhwang-San by high performance liquid chromatography (HPLC). And we predicted inhibition activity of major compounds of Gami-Samhwang-San using Quantitative Structure Activity Relationships (QSAR) Methods: The separation was performed on a YMC J,sphere-H80 CI8(250${\times}$4.6 mm I.D) column by gradient elution with $H_3PO_4$ buffers in acetonitrile as the moblie phase at a flow-rate of 1.0ml/min. Results: HPLC was employed to determine the quantities and the qualities of several marker substances such as ephedrine, pseudoephedirne, baicalin, ${\beta}-asarone$, tenuifoliside, naringenin, amygdalin and hyperoside in the SH-21-B. Conclusion: We suggest this results could be a useful evidence for quality control of SH-21-B.

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Optimization of an extraction method for the simultaneous quantification of six active compounds in the aril part of Orostachys japonicus using HPLC-UV

  • Gao, Dan;Kim, Jin Hyeok;Cho, Chong Woon;Yang, Seo Young;Kim, Young Ho;Kim, Hyung Min;Kang, Jong Seong
    • 분석과학
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    • 제34권4호
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    • pp.153-159
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    • 2021
  • In this study, we describe the development of a new high-performance liquid chromatography (HPLC) method for the simultaneous analysis of six bioactive compounds (including gallic acid, epicatechin 3-gallate, quercitrin, afzelin, quercetin, and kaempferol) from Orostachys japonicus. The extraction method was investigated and optimization of the extraction time (min), solvent composition (%), and solvent to material ratio were conducted. As a result, 30 min extraction with 50% methanol and 40:1 mL/g of solvent: material ratio achieved the highest extraction efficiency with a yield of 3.32 mg/g. Furthermore, the developed HPLC method was validated and the correlation coefficient (R) values were within the satisfactory range of 0.9995-0.9999 over the linearity range of 1.53-417 ㎍/mL. The limit of detection and limit of quantification for the six active components were between 0.03-0.08 ㎍/mL and 0.08-0.26 ㎍/mL, respectively. With these newly optimized and developed methods, four batches of O. japonicus were analyzed to confirm the high extraction efficiency of the method and the feasibility of an application.

GC/MS and HPLC/PDA characterization of essential oils and phenolic compounds from the aerial parts of common rue (Ruta graveolens)

  • Chang-Dae Lee;Hak-Dong Lee;Yunji Lee;Hwan Myung Lee;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • 제66권
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    • pp.144-152
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    • 2023
  • Two different extraction methods were used to evaluate the medical value of common rue, Ruta graveolens L. (RGL). The results of our 2,2-diphenyl-1-picrylhydrazyl and 2,2'-azino-bis-3-ethylbenzothiazoline-6-sulphonic acid assays indicated that the antioxidant activity of RGL essential oil extract obtained through steam distillation was very low, whereas ethanol (EtOH) extracts of RGL showed higher antioxidant activity. RGL essential oil was extracted by steam distillation and characterized by GC/MS analysis. Furthermore, EtOH extracts of RGL were obtained under reflux and analyzed by HPLC/PDA. The GC/MS results indicated that the ketone compounds 2-undecanol acetate, nonyl cyclopropanecarboxylate, and 2-nonanone accounted for more than 70% of the composition of RGL essential oil. The HPLC/PDA analyses indicated that the RGL extracts were rich in phenolic compounds such as protocatechuic acid, rutin, psoralen, xanthotoxin, and bergapten, among which rutin was the most abundant. Collectively, our results demonstrated that RGL contains high levels of phenolic compounds and could thus be commercialized as a valuable plant-derived antioxidant.

A Comparison of Analytical Methods for the Content and Purity of Cefradine

  • Hyun, Myung-Ho;Jeong, Euh-Duck;Shin, Min-Seob;Jin, Jong-Sung
    • Bulletin of the Korean Chemical Society
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    • 제29권6호
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    • pp.1185-1189
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    • 2008
  • Two HPLC methods such as cefadroxil and cefalexin methods were compared in their performance for the quantitative analysis of the content and purity of $\beta$ -lactamic antibiotic, cefradine, for six bulk drug samples. Between the two methods, the cefadroxil method prescribed by the European Pharmacopoeia (EP) for the determination of impurities in cefradoxil was superior to the cefalexin method prescribed by the EP and by the United States Pharmacopeia (USP) for the determination of cefalexin impurity in cefradine in terms of the greater stability of the chromatogram baselines and the higher precision, i.e., the lower % relative standard deviation (RSD). Based on the comparison of the two HPLC methods, the cefadroxil method was recommended to replace the TLC method, which has been prescribed by the EP as the official method for determination of extraneous impurities in cefradine.

봉독침의 봉독함량분석과 LD50 및 조직학적 소견 관찰 (Experimental Studies of quantitative evaluation using HPLC and safety of Bee Venom Acupuncture)

  • 장성봉;권기록
    • 대한약침학회지
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    • 제9권1호
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    • pp.155-165
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    • 2006
  • Objectives : This study was conducted to carry out quantitative evaluation and safety of Bee Venom Acupuncture. Methods : Content analysis was done using HPLC, measurement of $LD_{50}$, and histological observations were made on the skin and muscles. Results : 1. According to HPLC analysis, each BVA-1 contained approximately $0.36{\mu}g$, and BVA-2 contained approximately $0.54{\mu}g$. But the volume of coating was so minute, slight difference exists between each needle. 2. LD50 of mouse with BVA-1 was 16 counts and this is equivalent to 640 needles/kg, making Bee Venom Acupuncture safe treatment apparatus. 3. Regardless of the number of needles, there was no sign of blood stasis or inflammation detected on the skin and muscle tissues. Conclusion : Above results indicate that the Bee Venom Acupuncture can complement shortcomings of syringe usage as a part of Oriental medicine treatment, but extensive researches should be done for further verification.

Analysis of Microtoxins in the Nakdong River Watershed

  • Park, Jung-Min;Lee, Jae-Jung;Hwang, Dong-Jin;Yang, Sang-Yong
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 2003년도 International Symposium on Clean Environment
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    • pp.99-102
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    • 2003
  • The different methods such as HPLC, indirect- and direct-ELISA were employed for the analysis of microtoxins and the results of each method were compared in terms of the detection limit and accurary. Three toxins, microcystin-RR, -LR and -YR were clearly separated by HPLC using 0.05 M methanol and phosphate buffer used as a solvent system. The calibration curves for the toxins were linear in the range of 5 ng to 50 ng. The standard curves for the immunoassay of microcystin obtained by direct and indirect ELISA are compared. The linear responses of inhibitions of binding by microcystin in the direct and indirect competitive ELISA were in the range of 10 ng to 1000 ng and 50 pg to 160 pg, respectively. Distribution of microtoxins at 11 sites in the Nakdong river and several lakes in Korea was also studied. The most dominant microcystin variant in the test sites was found to be microcystin-RR.

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