• Title/Summary/Keyword: 분석법 검증

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Improvement and Validation of an Analytical Method for Quercetin-3-𝑜-gentiobioside and Isoquercitrin in Abelmoschus esculentus L. Moench (오크라 분말의 Quercetin-3-𝑜-Gentiobioside 및 Isoquercitrin의 분석법 개선 및 검증)

  • Han, Xionggao;Choi, Sun-Il;Men, Xiao;Lee, Se-jeong;Jin, Heegu;Oh, Hyun-Ji;Cho, Sehaeng;Lee, Boo-Yong;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.37 no.2
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    • pp.39-45
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    • 2022
  • This study aimed to investigate the validation and modify the analytical method to determine quercetin-3-𝑜-gentiobioside and isoquercitrin in Abelmoschus esculentus L. Moench for the standardization of ingredients in development of functional health products. The analytical method was validated based on the ICH (International Conference for Harmonization) guidelines to verify the reliability and validity there of on the specificity, linearity, accuracy, precision, detection limit and quantification limit. For the HPLC analysis method, the peak retention time of the index component of the standard solution and the peak retention time of the index component of A. esculentus L. Moench powder sample were consistent with the spectra thereof, confirming the specificity. The calibration curves of quercetin-3-𝑜-gentiobioside and isoquercitrin showed a linearity with a near-one correlation coefficient (0.9999 and 0.9999), indicating the high suitability thereof for the analysis. A. esculentus L. Moench powder sample of a known concentration were prepared with low, medium, and high concentrations of standard substances and were calculated for the precision and accuracy. The precision of quercetin-3-𝑜-gentiobioside and isoquercitrin was confirmed for intra-day and daily. As a result, the intra-day precision was found to be 0.50-1.48% and 0.77-2.87%, and the daily precision to be 0.07-3.37% and 0.58-1.37%, implying an excellent precision at level below 5%. As a result of accuracy measurement, the intra-day accuracy of quercetin-3-𝑜-gentiobioside and isoquercitrin was found to be 104.87-109.64% and the daily accuracy thereof was found to be 106.85-109.06%, reflecting high level of accuracy. The detection limits of quercetin-3-𝑜-gentiobioside and isoquercitrin were 0.24 ㎍/mL and 0.16 ㎍/mL, respectively, whereas the quantitation limits were 0.71 ㎍/mL and 0.49 ㎍/mL, confirming that detection was valid at the low concentrations as well. From the analysis, the established analytical method was proven to be excellent with high level of results from the verification on the specificity, linearity, precision, accuracy, detection limit and quantitation limit thereof. In addition, as a result of analyzing the content of A. esculentus L. Moench powder samples using a validated analytical method, quercetin-3-𝑜-gentiobioside was analyzed to contain 1.49±0.01 mg/dry weight g, while isoquercitrin contained 1.39±0.01 mg/dry weight g. The study was conducted to verify that the simultaneous analysis on quercetin-3-𝑜-gentiobioside and isoquercitrin, the indicators of A. esculentus L. Moench, is a scientifically reliable and suitable analytical method.

Development and Validation of Analytical Method and Antioxidant Effect for Berberine and Palmatine in P.amurense (황백의 지표성분 berberine과 palmatine의 분석법 개발과 검증 및 항산화 효능 평가)

  • Jang, Gill-Woong;Choi, Sun-Il;Han, Xionggao;Men, Xiao;Kwon, Hee-Yeon;Choi, Ye-Eun;Park, Byung-Woo;Kim, Jeong-Jin;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.35 no.6
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    • pp.544-551
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    • 2020
  • The aim of this study was to develop and validate a simultaneous analytical method for berberine and palmatine, which are representative substances of Phellodendron amurense, and to evaluate the antioxidant activity. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for berberine and palmatine using high-performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for berberine and palmatine exhibited 0.9999. The LODs for berberine and palmatine were 0.32 to 0.35 µg/mL and the LOQs were 0.97 to 1.06 µg/mL, respectively. The inter-day and intra-day precision values for berberine and palmatine were from 0.12 to 1.93 and 0.19 to 2.89%, respectively. The inter-day and intra-day accuracies were 98.43-101.45% and 92.39-100.60%, respectively. In addition, the simultaneous analytical method was validated for the detection of berberine and palmatine. Moreover, we conducted FRAP and NaNO2 scavenging activity assays to measure the antioxidant activities of berberine and palmatine, and both showed antioxidant activity. These results suggest that P.amurense could be a potential natural resource for antioxidant activity and that the efficacy can be confirmed by investigating the content of the berberine and palmatine.

Validation and Uncertainty Evaluation of an Optimized Analytical Method Using HPLC Applied to Canthaxanthin, a Food Colorant (식품 색소 Canthaxanthin의 HPLC 최적 분석법 확인 및 타당성과 측정불확도 평가)

  • Suh, Hee-Jae;Kim, Kyung-Su;Hong, Mi-Na;Lee, Chan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.3
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    • pp.342-351
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    • 2016
  • This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

Analysis of coenzyme Q 1O in dietary supplement by HPLC (HPLC를 이용한 건강기능식품 중 코엔자임 Q10 성분 분석)

  • No, Ki-Mi;Leem, Dong-Gil;Kim, Mi-Gyeong;Park, Kyoung-Sik;Yoon, Tae-Hyung;Hong, Jin;Park, Sun-Young;Jeong, Ja-Young
    • Journal of Food Hygiene and Safety
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    • v.26 no.1
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    • pp.12-15
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    • 2011
  • A method based on high-performance liquid chromatography (HPLC) with ultraviolet detection has been developed to quantify coenzyme Q10 (CoQ10) in raw materials and dietary supplements. Single-laboratory validation has been performed on the method to determine linearity, selectivity, accuracy, limits of quantification (LOQ) and repeatability for CoQ10. An excellent linearity (r=0.999) was observed for CoQ10 in the concentration range $15.625{\sim}500\;{\mu}g/ml$ in dietary supplement. Observed recovery of CoQ10 was found to be between 98.33 and 99.38%. LOQ was found to be $250\;{\mu}g/ml$ Repeatability precision for CoQ10 was between 0.15 and 0.21% relative standard deviation (RSD). Further, limited studies showed that some adulterants and degraded material could be satisfactorily separated from CoQ10 and identified.

An Empirical Study on the Activation Approach for the Competitive Power of Korean Shipping Company in the Korea-China Liner Routes (국적선사의 경쟁력 강화를 위한 한중정기항로 활성화 방안에 대한 실증연구)

  • Lee, Yong-Ho
    • Journal of Navigation and Port Research
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    • v.27 no.2
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    • pp.163-170
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    • 2003
  • This empirical study takes the activation approach for the competitive power of Korean shipping companies in the Korea-China liner routes. Data for this study were collected from Korea/ China/ 3rd flag shipping companies through the 500 questionnaires. The data of 250 respondents were analyzed statistically to verify the hypotheses and to induce Regression Equation which could predicts the influencing level of the determinants to competitive advantage for Korean shipping companies on Korea-China Liner Shipping Routes. Factor Analysis/ Cronbach's Alpha/ Principal Analysis/ Multiple Regression Analysis were used in order to test the hypotheses for the empirical study.

Selecting Technique of Accident Sections using K-mean Method (K-평균법을 이용한 고속도로 사고분석구간 분할기법 개발)

  • Lee, Ki-Young;Chang, Myung-Soon
    • International Journal of Highway Engineering
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    • v.7 no.4 s.26
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    • pp.211-219
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    • 2005
  • A selection of the analysis section for traffic accidents is used to analyze definitely the cause of accidents sorting similar accidents by a group and to raise the effect of improvement projects deciding the priority of accidents. In the existing method, an uniformly dividing method based on road mileages has been used, which has no consideration for similarities among accidents. Consequently, in recent, a slider-length method considering accident types rather than road mileages is widely used. In this study, using K-mean method, a non-hierarchical grouping technique used in the Cluster Analysis ai a applicatory method for the slider length method, a method classifies accidents that occurred the most nearby mileages into one group is proposed. To verify the proposed method, a comparison between the f-mean method and the dividing method at regular intervals on the data of a total of 25.6km lengths along Kyung-bu freeway in Pusan direction was made so that the K-mean method was proved to an effective method considering the similarities and adjacencies of accidents.

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Detecting Space-Time Clusters in Linear Point Data (선형 점자료에 있어서의 시.공 복합 군집의 탐색)

  • 홍상기
    • Journal of the Korean Geographical Society
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    • v.33 no.2
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    • pp.325-338
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    • 1998
  • 본 연구에서는 시.공 복합적인 선형 점 자료를 대상으로 시간과 공간을 함께 고려했을 때 자료 내에 군집(cluster)-시.공 복합 군집(space-time cluster)-이 존재하는 가를 검증하는 방법에 대해 논의하고, 실제 교통사고지점의 분포자료를 분석하여 군집의 유무를 통계적으로 검증하였다. 통계 분석의 결과 다음과 같은 사실이 확인되었다. 첫째, Knox의 분할표 방법과 Mantel의 역수 변환을 이용한 일반화된 회귀분석방법 모두 임계 거리 및 임계 시간 간격의 선택이 분석결과에 영향을 미친다. 둘째, 이러한 임의성을 극복하기 위해 다양한 임계 거리 및 임계 시간 간격(혹은 부가 상수)에 대해 반복 실험한 결과, 일부 임계값의 조합에서 시간과 공간이 서로 독립적이라는 귀무가설을 기각할 수 있는 증거가 발견되었다. 셋째, 시.공 복합 군집의 파악에 가장 적합한 임계 거리와 임계 시간 간격은 공간적으로는 7000m, 시간적으로는 14일 혹은 21일이다. 마지막으로, 통계 분석과정에서 자료에 존재하는 중복 기록 사고들의 존재가 밝혀짐으로써 시.공 복합군집 검증이 탐험적 자료 분석(exploratory data analysis)의 도구로서 가지는 가치를 확인할 수 있었다.

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Development of high performance liquid chromatography assay method of diosmin capsules (디오스민 캡슐의 HPLC 분석법의 개발)

  • Shim, Dae Hyun;Shin, Dong Han;Truong, Quoc Ky;Mai, Xuan Lan;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.29 no.6
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    • pp.277-282
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    • 2016
  • British Pharmacopoeia (BP 2013), the United States Pharmacopoeia (USP 39) and the Korean Pharmacopoeia (KP XI) contain monographs for the quality control of raw diosmin using high performance liquid chromatography (HPLC). However, official monographs detailing pharmaceutical formulations for diosmin are not available in foreign pharmacopoeias. In the KP XI, ultraviolet-visible (UV-Vis) spectroscopy-which is less specific than HPLC-is reported for the testing of diosmin capsules. In this study, we present an alternative HPLC assay for such testing that is more specific than UV-Vis methods. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2$>0.999), while the RSDs for intra- and inter-day precision were 0.15-0.29 % and 1.05-1.74%, respectively. Accuracies ranged from 101.2-103.2 %, while the retention time and peak area RSDs were 0.37 % and 0.06 %, respectively. Additionally, the plate number and asymmetry factor values for diosmin were 3591.293 and 1.35, respectively. Since the intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

Confirmation of Schizandrin as a Marker Compound in Jangsu Omija Powder (HPLC를 이용한 기능성 원료 지표성분으로서 장수 오미자 분말 중 Schizandrin의 분석법 개발)

  • Kim, Yunjeong;Ha, Na;Han, Song-Hee;Jeon, Ji-Young;Hwang, Minho;Im, Yong-Jin;Lee, Sun Young;Chae, Soo-Wan;Kim, Min-Gul
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.2
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    • pp.244-248
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    • 2013
  • We studied the development of schizandrin as a marker compound in Jangsu Omija. Schizandrin was validated for its LOD (limit of detection), LOQ (limit of quantitation), precision, accuracy, and recovery by HPLC relative to Omija powder. It showed a high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9990. The LOD and LOQ were 0.2 ${\mu}g/mL$ and 0.5 ${\mu}g/mL$, respectively. The intra- and inter-day precision of schizandrin calibration standards was 0.06~0.66% and 0.13~1.19%, respectively, and the intra- and inter-day accuracy of schizandrin was 98.35~103.30% and 98.35~103.00%, respectively. Overall, schizandrin was validated through our analytical methods as a marker compound in Jangsu Omija.

A Volume-Delay Function Parameter Estimation and Validation for Traffic Assignment (도로 통행지체함수의 파라미터 추정 및 검증)

  • Lim, Yong-Taek;Kang, Min-Gu;Choo, Sang-Ho;Lee, Sang-Min
    • Journal of Korean Society of Transportation
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    • v.26 no.3
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    • pp.17-29
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    • 2008
  • A volume-delay function(VDF) has been used to describe the relation between traffic volumes and delay experienced by travelers on the roads traveling from origin to destination, which has been usually adopted in traffic assignment. For the purpose of more precise description of traffic pattern, we have to estimate the parameters of VDF in advance. This paper presents a methodology for estimating the parameters, which combined with golden section method. By using the method we have estimated the parameters with real data based on KTDB(2006), and validated them. Compared to the existing values of the parameters, newly estimated values are found to be closer to real world.