• 한국의류학회지
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• 제37권6호
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• pp.827-836
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• 2013

Indigotin, indirubin, berberine, palmatine, alizarin, and purpurin are major pigments of indigo plant, Phellodendron bark, and madder. The six pigments were examined using the HPLC-DAD-MS instrument for the purpose of the simultaneous detection of the pigments in a single sample run. The HPLC-DAD-MS method examined the individual pigment solutions in DMSO, a solution containing 6 pigments, and the DMSO extract of the silk dyed with a dye solution of 5 pigments excluding indirubin. The retention times of the HPLC chromatograms, ${\lambda}_{max}$ of the uv-vis absorption bands in the DAD analyses, and the molecular ions detected for the compound peaks in the MSD analyses were consistent throughout the analyses of individual pigment solutions, mixed pigment solutions, and dye extracted from silk dyeing. The developed instrumental method of the simultaneous detection of six pigments can identify dye in an exhumed textile if the textile is dyed using any one (or multiple) pigments of indigo, Phellodendron bark, or madder plant.

• 한국국제농업개발학회지
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• 제30권4호
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• pp.339-346
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• 2018

본 연구는 HPLC-DAD/MS를 이용하여 농산물 중 triazine계 제초제인 cyanazine의 잔류 분석법을 확립하였다. 대표 농산물은 사과, 배추, 고추, 현미 및 콩을 선정하였고, 아세톤을 첨가하여 추출된 cyanazine 성분을 dichloromethane 액-액 분배법과 florisil 흡착크로마토그래피법으로 정제하여 HPLC-DAD/MS 분석대상의 시료로 사용하였다. Cyanazine의 정량적 분석을 위한 최적 HPLC-DAD/MS 분석조건을 확립하였으며, 정량한계(LOQ)는 0.02 mg/kg 이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과, 모든 처리농도에서 83.6~93.3% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 2.8%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였고, 또한 LC/MS SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 cyanazine의 HPLC-DAD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다.

• Natural Product Sciences
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• 제19권1호
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• pp.20-27
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• 2013

A simple high performance liquid chromatography - diode array detector (HPLC-DAD) method has been developed and validated for simultaneous determination of the six components (cinnamic acid, cinnamaldehyde, eugenol, atractylenolide I, atractylenolide III, and ergosterol) in Oryeongsan. In addition, identification of six marker compounds was conducted by a LC-MS/MS analysis. The six compounds in Oryeongsan were separated on Shishedo $C_{18}$ column (5 ${\mu}m$, $4.6{\times}250$ mm) at a column temperature of $30^{\circ}C$. The mobile phase was a mixture of 0.1% trifluoroacetic acid (TFA) water and acetonitrile employing gradient elution at a flow rate of 1.0 mL/min. The detection wavelength was set at 205, 250, 280, and 330 nm. The developed method had good linearity ($R^2$ > 0.9997) and the limit of detection (LOD) and limit of quantification (LOQ) were observed within the ranges 0.01~0.15 and 0.05~0.45 ${\mu}g/mL$, respectively. The relative standard deviation (RSD) values of intra- and inter-day testing were indicated that less than 3% and 90.31~103.31% of accuracy. The results of recovery test were 90.56~106.72% and RSD range was measured from 0.84 to 2.95%. In conclusion, this HPLC-DAD method has been successfully applied to the simultaneous determination of six compounds in Oryeongsan samples.

• 약학회지
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• 제52권6호
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• pp.446-451
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• 2008

A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of chlorogenic acid (1), sweroside (2), luteolin-7-O-glucoside (3), (E)-aldosecologanin (4) and 3,5-dicaffeoylquinic acid (5) from Lonicera joponica flower buds. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, 4.6${\times}$150 mm) with the column temperature $25^{\circ}C$. The mobile phase was composed of (A) water with 0.1% formic acid and (B) acetonitrile with 0.1% formic acid using a gradient elution, the flow rate was 0.3 ml/min. Detection wavelength was set at 250 nm. All calibration curves showed good linear regression ($r^2$>0.994) within test ranges. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.05${\sim}$1.95% and 0.15${\sim}$2.26%, respectively, and the overall recoveries of 97.71${\sim}$103.65% for the five compounds analyzed. The verified method was successfully applied to quantitative determination of the three types (phenolic compounds, iridoids and flavonoids) of bioactive compounds in 21 commercial L. japonica flower buds samples from different markets in Korea and China. The analytical results demonstrated that the contents of the five analytes vary significantly with sources.

• 한국염색가공학회지
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• 제32권4호
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• pp.255-264
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• 2020

With the development of synthetic dyes, excellent dyeing properties and massive production became possible. On the other hand, natural dyeing technology has gradually disappeared. However, the international environmental and human safety requirements of the apparel and textile industry are increasing, and there is a growing interest in safer and more environmentally friendly products. Accordingly, the public's interest in natural dyeing is increasing. To meet these demands, it is first necessary to clarify the stages of production and distribution of natural dyes. It is necessary to evaluate whether the product is a natural dye product and study the suitability of the natural dye product through qualitative and quantitative assessment of the indicator components of the natural dye. Typical of three natural dyes did qualitative and quantitative analysis by HPLC-DAD and HPLC-MS. Products dyed using natural dye three products were analyzed, and the presence or absence of detection of each indicator components was confirmed to confirm whether the product was dyed using natural dyes.

• 약학회지
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• 제54권3호
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• pp.157-163
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• 2010

A high-performance liquid chromatography (HPLC) with DAD detector and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of coniferin (1), loganic acid (2), demethylsecologanol (3), sweroside (4) and loganin (5) from caulis Lonicera joponica. The optimal chromatographic conditions were obtained on an ODS column ($5{\mu}m$, $4.6{\times}150mm$) with the column temperature $35^{\circ}C$. The mobile phase was composed of (A) water with 0.1% formic acid and (B) methanol with 0.1% formic acid using a gradient elution, the flow rate was 0.3 ml/min. Detection wavelength was set at 254 nm. All calibration curves showed good linear regression ($r^2$>0.998) within test ranges. The developed method provided satisfactory precision and accuracy with overall intra-day and interday variations of 0.16~3.28% and 0.14~1.99%, respectively, and the overall recoveries of 99.39~105.89% for the five compounds analyzed. The verified method was successfully applied to quantitative determination of the two types (phenolic compounds and iridoids) of bioactive compounds in 24 commercial caulis L. japonica samples from different markets in Korea and China. The analytical results demonstrated that the contents of the five analytes vary significantly with sources.

• Natural Product Sciences
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• 제22권4호
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• pp.238-245
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• 2016

Gumiganghwal-tang has been used for the treatment of common cold for a long-time. We developed an accurate and sensitive high performance liquid chromatography-diode array detection (HPLC-DAD) and electrospray ionization mass spectrometry method for the simultaneous determination of ferulic acid, baicalin, bergapten, methyl eugenol, glycyrrhizin, oxypeucedanin, wogonin, nodakenin, atractylenolide III, imperatorin, and atractylenolide I in Gumiganghwal-tang samples. The analytes were separated on a Shiseido C18 column ($5{\mu}m$, $4.6mm\;I.D.{\times}250mm$) with gradient elution with acetonitrile and 0.1% trifluoroacetic acid. Eleven compounds were quantitatively determined by HPLC-DAD and identified by LC-MS data. We also validated this method. The calibration curves of all the compounds showed good linear regression. The limits of detection and the limits of quantification ranged from 0.04 to 0.63 and from 0.12 to $1.92{\mu}g/mL$, respectively. The relative standard deviation values of intra- and inter-days of this method represented less than 2.9%. The recoveries were found to be in the range of 90.06 - 107.66%. The developed method has been successfully applied to the analysis of Gumiganghwaltang samples. The established HPLC method could be used to quality control of Gumiganghwal-tang.

• 분석과학
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• 제19권6호
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• pp.519-528
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• 2006

본 연구에서는 뇨시료를 고체상 추출법으로 추출한 후 HPLC/DAD/ESI-MS(high-performance liquid chromatograph/diode array detector/electro-spray ionitation mass spectrometry)를 사용하여 분석하였다. 7종의 thyroid hormones의 HPLC 분리조건은 Hypersil ODS(octadecylsilica) 컬럼(4.6mm I.D., 100 mm length, particle size $5{\mu}m$)을 사용하고 ammonium formate buffer와 acetonitrile을 이동상으로 하여 기울기 용리한 결과 완전 분리가 가능하였으며, UV spectra 및 질량스펙트럼을 확인할 수 있었다. 고체상 추출법에 의한 전처리 최적 조건을 조사한 결과 시료를 pH 3으로 한 후 C18 고체상을 사용하여 4 mL의 methanol/ammonium hydroxide(9:1) 혼합용액으로 용리할 경우 회수율이 89.0-113.1%로 나타났다. HPLC/DAD를 이용하여 10-1000 ng/mL범위에서 검량선을 작성한 결과 $r^2$값은 0.992-0.998 으로 나타났으며 검출한계는 2-4 ng/mL(3.8-13.0 pmol/mL)로 계산되었다.

• 한국자원식물학회지
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• 제30권6호
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• pp.693-698
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• 2017

The quality control of natural products is principal key to guarantee the Good Manufacturing Practices (GMP) and Good Clinical Practices (GCP) for the functional food, pharmaceuticals and cosmeceuticals in the industry. In this study, we examined the quantitative analysis of berberine as marker substance of Coptidis Rhizoma by high performance liquid chromatography-photodiode array detector (HPLC-DAD). The HPLC method was validated and met all the requirements for the quality control analysis recommended by FDA and ICH. The berberine was separated on a Xterra $C_{18}$ column ($5{\mu}m$, $4.6{\times}250mm$) using mobile phase consisting of distilled water and acetonitrile with $KH_2PO_4$ (3.4 g) and $Na_2SO_4$ (1.7 g). Calibration curve of berberine has been estimated (y = 42293.47x-41589 with the correlation coefficient 0.9999). The amount of berberine was calculated as 4.25%. And berberastine, palmatine, columbamine, jatrorrhizine, epiberberine, berberine and coptisine in the Coptidis Rhizoma were identified by high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-ESI-MS) method.

• Natural Product Sciences
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• 제16권3호
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• pp.164-168
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• 2010

High-performance liquid chromatographic method with diode-array detector and electrospray ionization with multi-stage tandem mass spectroscopy (HPLC/DAD/ESI-$MS^n$) was used to identify the major constituents in a methanolic extract of Eclipta prostrata. The chromatographic separation was performed on a C18 column. Acetonitrile-water was used as a mobile phase. HPLC/DAD/ESI-$MS^n$ allowed the characterization of constituents of E. prostrata, mainly triterpenoids (eclalbasaponin I, II, III, IV, VI), flavonoids (luteolin 7-O-glucoside, demethylwedelolactone, wedelolactone, luteolin, demetylwedelolactone sulfate, luteolin sulfate, apigenin sulfate) and phenolic acids (5-O-caffeoylquinic acid, 3, 4-O-dicaffeoylquinic acid, 3, 5-O-dicaffeoylquinic acid, 4, 5-Odicaffeoylquinic acid).