• 분석과학
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• 제28권3호
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• pp.168-174
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• 2015

남조류 독소인 마이크로시스틴은 여름철 우리나라 여러 호수들에 존재하여 물고기와 가축 그리고 인간에게 강한 독성을 나타내는 독소이다. 본 논문에서는 이러한 수중 남조류 독소, 마이크로시스틴을 정량분석하는 두가지 방법, 즉 고성능 액체크로마토그래피(HPLC) 분석법과 최근 우리 실험실에서 개발한 스트립분석법의 비교를 시도하였다. 두 분석법의 측정가능농도범위가 많이 달라 HPLC 법으로 먼저 측정한 후 시료를 물로 희석시켜 스트립분석법에 적용하였다. 서로 다른 농도의 마이크로시스틴을 함유한 7가지 물시료들을 사용하여 HPLC분석법과 스트립 분석법으로 남조류 독소 총량을 측정하였다. 그 결과 두 분석법의 정량측정결과가 매우 잘 일치하는 것을 볼 수 있었다. 두 분석법의 상관분석 결과 r 값은 0.99998 이었으며 통계적인 유의성을 나타내는 p 값은 0.00001 이었다.

• 생약학회지
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• 제40권2호
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• pp.103-108
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• 2009

GCSB-5 preparation is a purified extract from a mixture of 6 medicinal plants(Acanthopanacis Cortex, Achyranthis Radix, Saposhnikoviae Radix, Cibotii Rhizoma, Glycine Semen Nigra, Eucommiae Cortex) that have been widely used for the treatment of various bone disorders. The aim of this study was to investigate HPLC analysis method and screening of standard compound on Saposhnikoviae Radix for quality standardization of a medicinal crude drug GCSB-5. Standard compound of Saposhnikoviae Radix was decided with cimifugin by isolation and instrumental analysis such as NMR. HPLC analysis method for the simultaneous determination of cimifugin was established for the quality control of the medicinal plants of Saposhnikoviae Radix species, GCSB-5 raw material and preparation. And validation of HPLC analysis methods were conformed for verification of HPLC methods by check to specificity, linearity, intra-day precision, inter-day precision and accuracy following ICH guideline.

• 생약학회지
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• 제51권1호
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• pp.78-85
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• 2020

In this study, we shortly introduced the HPLC method validation guideline for the analysis of functional food which was released from the Ministry of Food and Drug Safety of Korea in Dec 2018. The HPLC method validation was performed through the aforementioned HPLC method validation guideline in order to quantitate scopoletin content from the hot-water extract powder of Artemisia annua Linné. The HPLC method was validated by evaluating specificity, accuracy, precision, limit of quantitation and linearity. All parameters were in the suitable ranges which are designated in the guideline, which indicated the current HPLC method is reliable to quantitate the scopoletin content from the hot-water extract of A. annua.

• 한국식품과학회지
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• 제32권4호
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• pp.788-791
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• 2000

키토올리고당의 정량법으로 기존의 비색법과 HPLC방법을 비교 검토하였다. HPLC에 의한 키토올리고당의 정량은 키토올리고당을 D-glucosamine로 분해한 다음, D-glucosamine을 분석하므로서 가능하였다. D-glucosamine를 분석하기 위한 HPLC 분석 조건은 검출기로서 RI detector 그리고 컬럼으로 Bondclone10 $NH_{2}$ column$(330{\times}3.9\;mm,\;10\;micron,\;Phenomenex)$을 사용하고 이동상으로는 acetonitrile : $H_{2}O$(65 : 35)으로 하였다. 키토올리고당의 정량은 비색법 보다 HPLC법이 높은 회수율을 보였으며, 분석시간도 시료당 10분 이내로서 비색법의 4 시간 보다 더 짧았다. 비색법은 키토산 등에 의한 false positive response가 일어났으나 HPLC법은 glucosamine 이외의 다른 성분에 의한 영향을 받지 않았다. 따라서 HPLC에 의한 키토올리고당의 정량은 가능하였으며 기존의 비색법 보다 신속 정확하였다.

• Natural Product Sciences
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• 제19권1호
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• pp.28-35
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• 2013

In this study, quantitative and pattern recognition analysis for the quality evaluation of Cinnamomi Ramulus and Cinnamomi Cortex using HPLC/UV was developed. For quantitative analysis, three major bioactive compounds were determined. The separation conditions employed for HPLC/UV were optimized using an ODS $C_{18}$ column ($250{\times}4.6$ mm, 5 ${\mu}m$) with gradient conditions of acetonitrile and water as the mobile phase, at a flow rate of 1.0 mL/min and a detection wavelength of 265 nm. This method was fully validated with respect to linearity, accuracy, precision, recovery, and robustness. The HPLC/UV method was applied successfully to the quantification of three major compounds in the extract of Cinnamomi Ramulus and Cinnamomi Cortex. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of thirty eight Cinnamomi Ramulus and thirty five Cinnamomi Cortex samples. The results indicate that the established HPLC/UV method is suitable for quantitative analysis.

• 대한본초학회지
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• 제28권5호
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• pp.95-101
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• 2013

Objectives : A quantitative method using high performance liquid chromatography with a photodiode array detector(HPLC-PDA) was established for the quantitative analysis of the four main compound and pattern analysis to classification Piiellia ternate, P. pedatisecta and Typhonium flagelliforme. Methods : The analytical procedure for the determination of P. ternata, together with the known main compounds uracil, uridine, guanosine and adenosine was established. Optimum HPLC-PDA separation of these P. ternata was possible on Luna C18(2) column material, using water and acetonitrile as mobile phase. The method was validated according to regulatory guidelines. In addition, this assay method were analyzed for the content of four main compound in P. ternata, P. pedatisecta and T. flagelliforme and by data obtained from the HPLC-PDA analysis was performed principal component analysis(PCA). Results : Validation results indicated that the HPLC method is well suited for the determination of the roots of P. ternata with a good linearity ($r^2$ > 0.999), precision and recovery rates. Analysis of HPLC-PDA, the average content of uracil, uridine, guanosine and adenosine was significantly higher in P. ternate>P. pedatisecta> T. flagelliforme order. The application of PCA to main compound data by HPLC-PDA permitted the effective discrimination among the three species. Conclusions : Analysis of both HPLC-PDA and PCA confirmed the fact that four main compound and pattern profiles of P. ternata, P. pedatisecta and T. flagelliforme were different from each other.

• 생명과학회지
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• 제23권2호
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• pp.306-310
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• 2013

본 연구는 요중 아플라톡신 M1 (AFM1)의 농도를 측정할 수 있는 competitive ELISA 방법의 특성을 HPLC-fluorescence detector (HPLC-FLD) 방법과 비교하여 평가하였다. ELISA 방법에서의 AFM1의 회수율은 105% (73-124%)였고 측정의 변이계수는 6.85%로 나타났다. ELISA 방법에서의 검출한계와 정량한계는 각각 0.20 pg/ml과 0.62 pg/ml로 조사되었으며, 두 방법을 이용하여 측정한 요중 AFM1 농도는 상관계수 0.96의 매우 높은 상관성이 있는 것으로 확인되었다(p<0.01). 그러나, 이렇게 높은 상관성에도 불구하고, ELISA 방법을 이용한 요중 AFM1의 농도는 HPLC-FLD 방법으로 측정한 값에 비해 상대적으로 높게 나타나는 경향을 보여 ELISA를 이용한 방법이 단시간에 많은 시료를 분석할 수 있는 장점은 있으나 그 결과는 HPLC-FLD 방법을 이용해서 얻은 회귀식을 이용하여 보정을 한 후 제시할 필요가 있는 것으로 판단된다.

• 한국수산과학회지
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• 제46권2호
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• pp.147-153
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• 2013

To prevent paralytic shellfish poisoning (PSP) due to the consumption of shellfish contaminated with PSP toxins, the quantitative analysis of these toxins is very crucial. The AOAC International mouse bioassay (MBA) has been used widely for the routine monitoring of PSP toxins for more than 50 years. However, this method has low sensitivity and high limit of quantification (LOQ) and interferences from other components in the extract, and it cannot determine toxic profiles. Ethical problems also exist with the continued use of this live mouse assay. To establish an alternative method to the MBA used for PSP toxins analysis, we attempted to optimize the analysis conditions of a precolumn high-performance liquid chromatography (HPLC) oxidation method and succeeded in validating its accuracy and precision in quantifying PSP toxins. A clear peak and the isolation of PSP toxins were obtained by injecting the working standards of Certified Reference Materials using HPLC. The LOQ of the precolumn HPLC oxidation method for PSP toxins was about $0.1002{\mu}g/g$, which represented an approximately fourfold improvement in detection capability versus the AOAC MBA. The intra-accuracy and precision for PSP toxins in oysters were 77.0-103.3% and 2.0-5.7%, respectively, while the respective inter-accuracy and precision were 77.3-100.7% and 2.4-6.0%. The mean recoveries of PSP toxins from oysters were 75.2-112.1%. The results of a comparison study showed good correlation between the results of the precolumn HPLC oxidation method and those of MBA, with a correlation factor of 0.9291 for mussels. The precolumn HPLC oxidation method may be used as an alternative to, or supplementary method with, MBA to monitor the occurrence of PSP toxins and to analyze the profiles of these toxins in shellfish.

• 생약학회지
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• 제41권1호
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• pp.48-53
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• 2010

GCSB-5 preparation is a purified extract from a mixture of 6 medicinal plants(Acanthopanacis Cortex, Achyranthis Radix, Saposhnikoviae Radix, Cibotii Rhizoma, Glycine Semen Nigra, Eucommiae Cortex) that have been widely used for the treatment of various bone disorders. The aim of this study was to investigate HPLC analysis method and screening of standard compound on Cibotii Rhizoma for quality standardization of a medicinal crude drug GCSB-5. Onitin-4-O-$\beta$-D-glucopyranoside was isolated from Cibotii Rhizoma as the standard compound and identified on the basis of spectroscopic data such as NMR. HPLC analysis method for the determination of onitin-4-O-$\beta$-D-glucopyranoside was established for the quality control of the medicinal plants of Cibotii Rhizoma species, GCSB-5 raw material and GCSB-5 preparation. And validation of HPLC analysis methods were conformed for verification of HPLC methods by check to specificity, linearity, intra-day precision, inter-day precision and accuracy following ICH guideline.

• Bulletin of the Korean Chemical Society
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• 제31권11호
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• pp.3371-3381
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• 2010

In this study, quantitative and pattern recognition analysis for the quality evaluation of Magnoliae Flos using HPLC/UV was developed. For quantitative analysis, eleven major bioactive lignan compounds were determined. The separation conditions employed for HPLC/UV were optimized using ODS $C_{18}$ column ($250{\times}4.6\;mm$, $5\;{\mu}m$) with isocratic elution of acetonitrile and water with 1% acetic acid as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 278 nm. These methods were fully validated with respect to the linearity, accuracy, precision, recovery, and robustness. The HPLC/UV method was applied successfully to the quantification of eleven major compounds in the extract of Magnoliae Flos. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of twenty one reference samples corresponding to seven different species of Magnoliae Flos and nine samples purchased from market. The results indicate that the established HPLC/UV method is suitable for the quantitative analysis and quality control of multi-components in Magnoliae Flos.