• 제목/요약/키워드: $k_0$-Standardization Method

검색결과 153건 처리시간 0.022초

정량분석을 통한 Eleutherococcus species의 HPLC 분석법 검증과 표준화 (Standardization of Eleutherococcus species and HPLC Method Validation for Quantitative Analysis)

  • 송미경;김미연;김호철
    • 대한본초학회지
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    • 제26권1호
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    • pp.103-110
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    • 2011
  • Objective : For the standardization and quality control of eleutheroside E in Eleutherococcus species, HPLC analysis was performed and eleutherosdie E content was compared in 23 kinds of Eleutherococcus species collected from Korea and China. Methods : The content of eleutheroside E in stem bark of Eleutherococcus species collected from Korea and China were analyzed by HPLC. 0.5% phosphoric acid and acetonitrile was used as mobile solvent. Validation of HPLC analysis method was confirmed by analyzing specificity, linearity, precision and accuracy following ICH guideline. Results : Content of eleutheroside E was determined to be 1.0-1.6% and 0.5-0.8% in Korean and Chinese E. senticosus, respectively. Content of eleutheroside E in E. sessiliflorus was 0.7-1.1% and 0.2-0.4% respectively in Korean and Chinese origin. All calibration curves showed good linear regression. The method showed good precision and accuracy with intra-day and inter-day variations of 0.880-3.442% (RSD) and 0.606-3.328% (RSD), respectively, and average recovery was of 0.141-1.363% (RSD), for the eleutheroside E analyzed. Conclusion : These results might be used to establish a criterion of eleutheroside E in Eleutherococcus species.

$k_0$-표준화방법에 의한 기기중성자방사화 분석법의 고찰 (The Review of Instrumental Neutron Activation Analysis by $k_0$-standardization method)

  • 문종화;정용삼;김선하
    • 분석과학
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    • 제14권4호
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    • pp.1075-1081
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    • 2001
  • 기기중성자방사화 분석법은 핵 분석기술의 대표적인 방법으로 비파괴-동시 다원소분석의 장점과 함께 절대측정값에 의해 정량 할 수 있다는 특징을 갖고 있다. 최근에는 정확도와 편의성을 만족할 수 있는 $k_0$-정량법을 사용한 기기중성자방사화 분석법이 세계적으로 일반화되고 있다. 본 연구에서는 $k_0$-법의 적용을 위하여 이 방법의 전체적인 개념의 소개와 함께 $k_0$-파라미터를 측정하고자 하였다. 이를 위하여 $k_0$-법의 개념이해와 정량에 필요한 인자들의 정의 및 파라미터인 $Q_0$(${\alpha}$)와 f 값을 결정하기 위한 수식과 실험적 측정방법 등을 요약하였고 중성자조사공에 따라 특성 값을 갖는 ${\alpha}$와 f 값을 하나로 연구용원자로의 방사화분석용 조사공(NAA#1)에서 측정하여 $k_0$-법의 도입을 위한 기반을 마련하였다.

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Method development and validation for dieckol in the standardization of phlorotannin preparations

  • Kim, Jiyoung;Um, Minyoung;Yang, Hyejin;Kim, Inho;Lee, Changho;Kim, Yuntai;Yoon, Minseok;Kim, Youngkyoung;Kim, Jimi;Cho, Suengmok
    • Fisheries and Aquatic Sciences
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    • 제19권1호
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    • pp.3.1-3.6
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    • 2016
  • Phlorotannins are reported to have diverse biological properties. However, no analytical methods for the standardization of phlorotannin preparations have been reported. Herein, we developed and validated an analytical method for the determination of dieckol in phlorotannin extracts (PRT) using high-performance liquid chromatography (HPLC). The optimum HPLC conditions consisted of a Supelco Discovery C18 column stationary phase, a mobile phase (A: 15 % HPLC grade methanol in deionized water, B: methanol), UV detection at 230 nm, and a flow rate of 0.7 mL/min. The optimized chromatographic conditions were validated and exhibited good specificity and linearity ($R^2$ > 0.9994-1.0000). The recoveries were in the range of 100.9-102.3 %. The method had good intermediate (%RSD 1.2) and intra-day (%RSD 0.4-1.7) assay precisions. This HPLC method had good accuracy and quality in the determination of dieckol in PRT.

플라스틱 소재의 비소 함유량 분석에 관한 연구 (Analytic study on arsenic content in plastic materials)

  • 이재인;최철호;최기인;고병례;최인석;조훈식
    • 분석과학
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    • 제25권6호
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    • pp.402-409
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    • 2012
  • 연속흐름 수소화물 생성-유도결합 플라스마 원자 방출 분광기(FI-HG-ICP-AES) 이용하여 플라스틱 소재에 함유된 비소를 정량하기 위한 조건을 얻었다. 플라스틱 시료를 습식 산 분해 방법 및 마이크로파 산 분해 방법으로 전처리하여 시험 용액을 조제하였다. 인증표준물질(CRM)인 CRM-EC680k 및 CRM-EC681k를 사용하여 측정한 값과 인증값을 비교하여 분석 방법의 재현성 및 정확성을 확인하였다. 습식 산 분해 방법 및 마이크로파 산 분해 방법으로 전처리하여 FI-HG-ICP-AES로 측정한 결과 CRM-EC680k의 경우에는 4.1~4.3 mg/kg (인증값 $4.1{\pm}0.5$ mg/kg)이고, CRM-EC681k의 경우에는 28.9~30.6 mg/kg (인증값 $29.1{\pm}1.8$ mg/kg)이었다.

배암차즈기 추출물의 기능성원료 표준화를 위한 지표성분으로서 Hispidulin의 분석법 평가 (Analytical Method for the Validation of Hispidulin as a Marker Compound for the Standardization of Salvia plebeia R. Br. Extracts as a Functional Ingredient)

  • 전윤정;곽호영;최종길;이제혁;최수임
    • 한국약용작물학회지
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    • 제24권4호
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    • pp.271-276
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    • 2016
  • Background: In the present study, we established an HPLC (high performance liquid chromatography)-analysis method for the determination of marker compounds as a part of the material standardization for the development of health-functional foods from Salvia plebeia R. Br. extract. Methods and Results: The quantitative determination method of hispidulin as a marker compound was optimized by HPLC analysis using a YMC hydrosphere C18 column with a gradient elution system. This method was validated using specificity, linearity, accuracy, and precision tests. It showed a high linearity in the calibration curve with a coefficient of correlation ($r^2$) of 0.999995. The method was fully validated, and was sensitive, with the limit of detection (LOD) at $0.09{\mu}g{\cdot}m{\ell}^{-1}$ and limit of quantification (LOQ) at $0.27{\mu}g{\cdot}m{\ell}^{-1}$. The relative standard deviation (RSD) values of the data from intra- and inter-day precision were 0.05 - 0.22% and 0.32 - 0.42%, respectively, and the intra- and inter-day accuracy of hispidulin were 99.5 - 102.3% and 98.8 - 101.5%, respectively. The average content of hispidulin in Salvia plebeia R. Br. extract was $3.945mg{\cdot}g^{-1}$ (0.39%). Conclusions: These results suggest that the developed HPLC method is very efficient, and that it could contribute to the quality control of Salvia plebeia R. Br. extracts as a functional ingredient in health functional foods.

판크레아틴의 규격 표준화 연구 (Standardization of Pancreatin)

  • 신지은;윤혜경;김동현
    • Journal of Pharmaceutical Investigation
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    • 제33권4호
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    • pp.273-279
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    • 2003
  • Pancreatin is a enzyme mixture breaking down carbohydrates, proteins and lipids. Most pancreatin used in Korea is imported from foreign countries. However, guideline of each country for pancreatin produced from each country is different. Therefore, guideline for pancreatin imported from several countries, such as Europe, Japan and America, it is standardized to control its quality. Assay of enzyme activity for pancreatin in KP is similar to tat in JP, but it is significantly different from those in FP ad in USP. We measured pancreatin digestive activities of 17 commercial products. Activity assay of digestive enzymes, starch- and lipid-digestive enzymes, for pancreatin by KP method (including JP) was difficult compared to those by FIP ad USP methods. Particularly, activity assays of starch- and lipid-digestive enzymes by KP method were mistakable, ad varied in diluted samples than those by FIP. However, activity assay of protein-digestive enzyme by KP method was similar to that by FIP. Starch-digestive enzyme activities of 17 commercial pancreatins by KP method were lower 0.079-fold compared to those by FIP method. Their protein-digestive enzyme activities by KP method were higher 75.7-fold than those by FIP method. Their lipid-digestive enzyme activities by KP method were lower 0.234-fold compared to those by FIP method.

UPLC-DAD를 이용한 불환금정기산의 다성분 동시분석법 개발 (Development of an UPLC-DAD Method for Simultaneous Analysis of Eight Marker Compounds of Bulhwangeumjeonggi-san)

  • 이경희;라미차네 라마칸타;서르마 디박 쿠마르;판데야 프라카스 라즈;김세건;정현주
    • 생약학회지
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    • 제47권4호
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    • pp.366-373
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    • 2016
  • Bulhwangeumjeonggisan (BHGJGS) is a traditional herbal formulation generally used in the treatment of cold and gastritis. BHGJGS consists of eight herbal plants; Atractylodis Rhizoma, Magnoliae Cortex, Citri Pericarpium, Glycyrrhizae Radix, Agastachis Herba, Pinelliae Rhizoma, Zingiberis Rhizoma and Zizyphi Fructus. Complete standardization of this formulation has not been done yet. So, a simple and accurate method was developed and validated using Ultra Performance Liquid Chromatography (UPLC) with Diode Array Detector (DAD) for the standardization of BHGJGS. UPLC conditions were optimized using a c18 RP-Amide column with mobile phase; 0.1% phosphate buffer and acetonitrile, detection wavelength; 210 and 325 nm. The linearities of calibration curves were acceptable ($R^2$>0.9994), and the limit of detection and quantification were within the ranges of 0.011-0.091 and $0.034-0.277{\mu}g/ml$ respectively. The relative standard deviation (RSD) of intra- and inter-day precisions were under 3.61%. The RSD of repeatability was under 0.68 %. The results of recovery test were 94.4-107.9%, and the RSD were under 4.6%. The developed method was used to find the contents of standard constituents in BHGJGS mix extract powder, and two commercial formulation (A and B). The data show that the developed method was specific, sensitive, accurate, and precise for analysis of BHGJGS components.

Establishment and Selection of Indicator Materials for Cervi Parvum Cornu Pharmacopuncture

  • Yang, Kyu-Jin;Lee, Ki-Beom;Kim, No-Hyeon;Kim, Tae-Gyu;Gi, Yu-Mi;Joo, Hwan-Soo;Suh, Chang-Yong;Lee, In-Hee;Chung, Hwa-Jin;Ha, In-Hyuk;Lee, Jae-Woong
    • Journal of Acupuncture Research
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    • 제34권4호
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    • pp.180-184
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    • 2017
  • Background: Recently, Cervi Parvum Cornu pharmacopuncture has been widely used. But no studies on the indicator materials for Cervi Parvum Cornu pharmacopuncture have been conducted. The aim of this study was to select indicator materials that would aid in the uniform preparation of standardized Cervi Parvum Cornu pharmacopuncture. Methods: Three lots of Cervi Parvum Cornu pharmacopuncture were analysed. Each lot was prepared using the same methods and materials. Chondroitin sulfate, alanine, and leucine were selected as the indicator materials for Cervi Parvum Cornu. For standardization, chondroitin sulfate analysis was performed using the colorimetric method, while alanine and leucine were analyzed using liquid chromatography-mass spectrometry (LC-MS). Results: Analysis of the three lots of Cervi Parvum Cornu pharmacopuncture found chondroitin sulfate levels of $108.9{\pm}17.3ug/ml$, $118.8{\pm}5.0ug/ml$ and $112.3{\pm}11.9ug/ml$. Alanine levels were $44.9{\pm}2.8ug/ml$, $44.6{\pm}0.3ug/ml$, and $43.9{\pm}0.2ug/ml$. Leucine levels were $29.6{\pm}0.7ug/ml$, $29.0{\pm}0.1ug/ml$, and $29.4{\pm}0.1ug/ml$. Conclusion: These results suggest that chondroitin sulfate, alanine, and leucine may be useful for the standardization of Cervi Parvum Cornu pharmacopuncture.

Assessment of Nuclear Characteristics of NAA #1 Irradiation Hole in HANARO Research Reactor for Application of the $K_0$-NAA Methodology

  • Moon, Jong-Hwa;Kim, Sun-Ha;Chung, Yong-Sam;Dung, Ho-Mahn
    • Nuclear Engineering and Technology
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    • 제34권6호
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    • pp.566-573
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    • 2002
  • Neutron activation analysis based on $textsc{k}$$_{o}$-standardization method# ($textsc{k}$o-NAA) is Com as one of the most remarkable progresses of the NAA with advantages of experimental simplicity, high accuracy, excellent flexibility with respect to irradiation and counting conditions, and suitability for computerization. This study was carried out to determine the reactor neutron spectrum parameters, i.e. $\alpha$ and f as the main factors of irradiation quality at NAA #1 irradiation hole on HANARO research reactor, to evaluate peak detection efficiency of the gamma-ray spectrometer for the use in the $textsc{k}$$_{o}$ experiments and to compare the measured concentration results with the certified values of some SRMs applying the experimentally determined to-parameters.ers.

기계적 충격기술을 적용한 멥쌀 경단의 규격 표준화 및 품질특성에 대한 연구 (Study on the Standardization and Physicochemical Property for Non-waxy Gyungdan Adapted with Mechanically Impacting Technology)

  • 한서영;박혜영;신동선;김경미;한귀정
    • 한국식품조리과학회지
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    • 제29권1호
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    • pp.29-36
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    • 2013
  • The present study was conducted to supply more scientific information for standardization of preparation method of Gyungdan and to determine the standard for manufacturing procedure adapted with mechanically impacting technology (MIT) for mass production. The optimum preparation condition for non-waxy Gyungdan adapted with MIT was 35% of water, 0.5% of wheat flour (w/w of soaked rice), and mechanically impacting for 10 min at 450 rpm. In the present study, standardization of manufacturing procedure for merchandizing of Gyungdan was established with width, weight, and height. Average of Gyungdan adapted with MIT at 90 rpm (stuffing speed) and 46.58 Herz (cutting speed) is 18.3 g of weight, 28.4 mm of height, and 32.4 mm of width. Hardness, as a main parameter of texture profile, of Gyungdan was maintained lower than 100 g up to 3 days at the storage of $20^{\circ}C$ and up to 70 days at the storage of $-20^{\circ}C$. And, it was performed to develop rice cake as meal-replacement adapted with MIT and sub-ingredients such as strawberry, pumpkin, and mugwort. Gyungdan prepared under controlling manufacturing condition of MIT was supplemented with 0-1.6% of sub-ingredients, respectively. In sensory tests, the best substitute ratios of strawberry, pumpkin, and mugwort were 1.6%, 0.8%, and 1.6%, respectively. With the results above, not-harden Gyungdan supplemented with sub-ingredients and various stuffs can be expected to application for wheat-substitute meal-replacement.