• 보존과학회지
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• 제31권3호
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• pp.299-308
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• 2015

본 연구는 1996년 천안시 유량동에서 출토된 분홍색 단령의 염료 동정을 통해 조선시대에 사용된 적색 염료를 실증하기 위한 것이다. 이를 위해 유물에 사용된 염료를 추출하고 이것을 당시 염색에 사용되었을 것으로 추정되는 적색계 염료(홍화, 소목, 꼭두서니)에서 추출한 염료와 함께 고성능액체크로마토그래피분석을 실시하였다. 그 결과 유물에서 추출한 염료와 홍화염색포의 추출 염료는 같은 시간대인 17.5분에서 피크가 나타났다. 이때 자외/가시선 분광 분석 결과는 두 시료 모두 519nm에서 최대흡수파장이 나타나 기존 홍화의 홍색소 분석 결과와 같은 것으로 조사되었다. 또한 negative ion mode에서 질량분석을 실시한 결과 유물과 홍화 염색포에서 추출한 염료 시료는 carthamin의 분자량인 910을 나타내는 m/z 909에서 같은 시간대의 피크가 확인되었다. 이와 같은 결과로 이 분홍 단령 직물을 염색하는데 사용된 염재는 홍화인 것으로 동정되었다.

• 생약학회지
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• 제41권4호
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• pp.313-318
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• 2010

Guibi-tang, a traditional herbal medicine, is used for anti-oxidant, anti-osteoporosis, hemostasis and gastroprotection. To develop an analysis method of simultaneous determination of six compounds, swertisin, decursinol, glycyrrhizin, 6-gingerol, costunolide and decursin in Guibi-tang, a high performance liquid chromatography was used with diode array detector. Six bioactive components were separated on a SHISEIDO $C_{18}$ column ($5\;{\mu}m$, 4.6 mm I.D.${\times}$250 mm) with column temperature $30^{\circ}C$. The gradient elution was composed of water with 0.1% trifluoroacetic acid (TFA) and acetonitrile. UV wavelength was set at 230 nm, 254 nm and 330 nm, respectively. Calibration curve showed good linear regression ($R^2$ > 0.9999). The limits of detection (LOD) and the limits of quantification (LOQ) ranged in 0.03 - 0.23 ${\mu}g/ml$ and 0.08 - $0.70\;{\mu}g/ml$, respectively. The RSD values of intra- and inter-day test were in the range of 0.03 ~ 0.96% and 0.01 ~ 1.46%, respectively. The evaluated results of accuracy test were varied from 92.28% ~ 105.14% with RSD < 1.60%. In conclusion, this developed simultaneous determination method was accuracy and sensitive to the quality evaluation of Guibi-tang.

• KSBB Journal
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• 제18권4호
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• pp.261-265
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• 2003

이부프로펜 중 S-enantiomer는 약물학적 효과를 갖고 있으나 R-enantiomer는 여러 가지 부작용을 갖고 있다. 이런 라세미 혼합물은 키랄 고성능 액체 크로마토그래피를 이용하여 효과적으로 분리 할 수 있었다. 실험에서 이용한 column(3.9 ${\times}$ 300 mm)은 Kromasil 10 $\mu\textrm{m}$를 충진하였고, 이동상으로는 n-hexane/tert-butyl methyl ether/acetic acid를 사용하였다. 유속은 1.0 $m\ell$/min 주입부피는 5 ${\mu}\ell$이고, UV 검출기의 wavelength는 220 nm이며 실온에서 실험하였다. 라세미 형태의 이부프로펜을 키랄 고정상으로 채워진 컬럼을 이용하여 이동상의 조성비를 바꿔가면서 이동상의 조성 변화에 따른 두 물질의 분리도의 상관식을 얻었다. 이 상관식을 이용하여 각 조성에 분리도에 미치는 영향을 정량적으로 표시하였고 보간법 또는 외사법에 의하여 실험이외의 조성에 대한 분리도를 예측할 수 있는 장점이 있다.

• Journal of Pharmaceutical Investigation
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• 제34권6호
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• pp.453-457
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• 2004

Atenolol and related compounds found in raw materials and commercial products were analyzed by reversed-phase high-performance liquid chromatography. A mixed solution of phosphate buffer (3.4 g/l, pH 3.0), tetrahydrofurane and methanol (800:20:180, v/v/v) including sodium octanesulfonate (1 g/l) and tetrabutylammonium-hydrogensulfate (0.4 g/l) was used as mobile phase at the flow rate of 0.25 ml/min. Detection was carried out at UV 226 nm. Atenolol related compounds, such as bis ether, tertiary amine and blocker acid were identified by comparing the retention time of the standard. The within-day and between-day precisions of the separated compounds were less than 1.2% and 3.4%, respectively. The contents of related compounds of the tested samples were under the limit prescribed in the European Pharmacopoeia. The pattern of the related compounds showed that atenolol raw materials and products could be classified in three different groups, indicating that the materials originated from different source or treated in different way.

• 한국자원식물학회지
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• 제31권6호
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• pp.652-659
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• 2018

In this study, baicalin, as a marker substance of Scutellariae Radix, was quantitatively analyzed by a high performance liquid chromatography-photodiode array detector (HPLC-DAD). We identified wogonoside, baicalein, and wogonin in the Scutellariae Radix by a high performance liquid chromatography-electrospray ionization-mass spectrometer (HPLC-ESI-MS). The baicalin was separated on a Xterra C18 column ($5{\mu}m$, $4.6{\times}250mm$) using mobile phase consisting of 38% acetonitrile in 0.68% phosphoric acid. The baicalin spectrum in the Scutellariae Radix extracts was coincided by comparing with UV-visible spectrum (200-550 nm) of baicalin standard in the library. The amount of baicalin in Scutellariae Radix was 10.46%, which is higher than KFDA's guideline. The marker substances of Scutellariae Radix showed a strong base peak $[M]^+$ in the positive detection mode following as; baicalin (m/z; $271[MH^+-sugar]^+$, $447[M+H]^+$), wogonoside (m/z; $285[MH^+-sugar]^+$, $461[M+H]^+$), baicalein (m/z; $271\;[M+H]^+$), wogonin (m/z; $285[M+H]^+$). These results are consistent with the fragment pattern and molecular weight of standard components from literature.

• 분석과학
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• 제32권4호
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• pp.139-146
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• 2019

A simple and reliable analytical method based on high-performance liquid chromatography-ultraviolet detection was established for the analysis of the flowers of Chrysanthemum morifolium (CM). Luteolin-7-O-glucoside (LU7G) was chosen as a target analyte considering its content, availability, and ease of analysis. Chromatographic separation of LU7G was achieved using a Phenomenex Gemini $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) run with a mobile phase consisting of 0.5 % acetic acid in water and 0.5 % acetic acid in acetonitrile at a flow rate of $1.0mL\;min^{-1}$. The detection wavelength and column temperature were set at 350 nm and $40^{\circ}C$, respectively. Method validation was performed according to the AOAC guidelines and the method was specific, linear ($R^2=0.9991$ for $50-300{\mu}g\;mL^{-1}$), precise (${\leq}3.91%$RSD), and accurate (100.1-105.7 %). The limits of detection and quantification were 3.62 and $10.96{\mu}g\;mL^{-1}$, respectively. The established method was successfully applied to determine the contents of LU7G in various batches of bulk CM extracts and labscale CM extract. The developed method is a readily applicable method for the quality assessment of CM and its related products.

• 분석과학
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• 제37권4호
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• pp.220-229
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• 2024

This study aims to developing a method for estimating pharmaceutical compounds within a monolith column using high-performance liquid chromatography (HPLC). The monolithic column was prepared using copolymerization of glycidyl methacrylate, co-ethylene dimethacrylate, and co-acrylic acid inside a borosilicate tube of specific dimensions a 60 mm borosilicate tube length with 1.5 mm and 3.5 mm inner and outer diameters, respectively. A UV Ultra violet source with a wavelength of 365 nm was used, and the polymerization process involved mixing glycidyl methacrylate, acrylic acid, ethylene dimethacrylate as a binder, and 2,2-dimethoxy-2-phenyl acetate phenone as an initiator in suitable solvents consisting of ethanol and 1-hexanol. The polymerization process formed the monolith column after 4 minutes, and subsequently, the epoxy groups were altered to diol groups using 0.2 M hydrochloric acid HCl, which were pumped through the column for 3 hours at a flow rate of 10 µL·min^-1. Various techniques, such as Scanning Electron Microscope SEM, Brunauer-Emmett-Teller BET, Fourier-transform infrared spectroscopy FT-IR and HNMR, were utilized to characterize and confirm the structure of the monolith. The prepared monolith was employed to estimate and identify the pharmaceutical compound of warfarin using high-performance liquid chromatography HPLC. The analytical curve of warfarin was linear in the range of 3 to 100 ㎍·mL^-1 with an r² value of 0.999. The detection and quantification limits were 0.932 and 2.788 ㎍·mL^-1, respectively. The molar absorptivity and Sandells sensitivity were 2.99138 × 10⁶ L·mol^-1·cm^-1 and 103.1 × 10^-3 ㎍·cm^-2, respectively.

• Toxicological Research
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• 제24권3호
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• pp.207-212
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• 2008

Pesticide residues play several key roles as environmental and food pollutants and it is crucial to develop a method for the rapid determination of pesticide residues in environments. In this study, a simple, effective, and sensitive method has been developed for the quantitative analysis of methoxyfenozide in water and soil when kept under laboratory conditions. The content of methoxyfenozide in water and soil was analyzed by first purifying the compound through liquid-liquid extraction and partitioning followed by florisil gel filtration. Upon the completion of the purification step the residual levels were monitored through high performance liquid chromatography(HPLC) using a UV absorbance detector. The average recoveries of methoxyfenozide from three replicates spiked at two different concentrations and were ranged from 83.5% to 110.3% and from 98.1% to 102.8% in water and soil, respectively. The limits of detection(LODs) and limits of quantitation(LOQs) were 0.004 vs. 0.012 ppm and 0.008 vs. 0.024 ppm, respectively. The method was successfully applied to evaluate the behavioral fate of a 21% wettable powder(WP) methoxyfenozide throughout the course of 14 days. A first-order model was found to accurately fit the dissipation of methoxyfenozide in water with and a $DT_{50}$ value of 3.03 days was calculated from the fit. This result indicates that methoxyfenozide dissipates rapidly and does not accumulate in water.

• KSBB Journal
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• 제26권4호
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• pp.323-327
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• 2011

The convenient derivatization method of chiral amino alcohols as 9-anthraldimine Schiff base derivatives for chiral resolution was developed and the liquid chromatographic enantiomer separation of chiral amino alcohols as 9-anthraldimine derivatives was investigated on several coated and covalently bonded polysaccharide-derived chiral stationary phases (CSPs). In general, the performance of Chiralcel OD-H (or Chiralcel OD) (${\alpha}$ = 1.24-2.89), the coated CSP derived from cellulose derivative was superior to the other CSPs for resolution of 9-anthraldimine derivatives of several amino alcohols. The results of enantioseparation depending on the structure of 9-anthraldimine analytes like the steric bulky group and the polar moiety etc were discussed. The analytical method was applied to measure the enantiomeric purity of commercially available chiral amino alcohols. It is expected that the convenient analytical method will be very efficient for determination of enantiomeric purity of amino alcohols as 9-anthraldimine Schiff base derivatives with strong UV absorption.

• 대한약침학회지
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• 제17권4호
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• pp.36-49
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• 2014

Objectives: Quercetin and curcuminoids are important bioactive compounds found in many herbs. Previously reported high performance liquid chromatography ultraviolet (HPLC-UV) methods for the detection of quercetin and curcuminoids have several disadvantages, including unsatisfactory separation times and lack of validation according the standard guidelines of the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. Methods: A rapid, specific, reversed phase, HPLC-UV method with an isocratic elution of acetonitrile and 2% v/v acetic acid (40% : 60% v/v) (pH 2.6) at a flow rate of 1.3 mL/minutes, a column temperature of $35^{\circ}C$, and ultraviolet (UV) detection at 370 nm was developed. The method was validated and applied to the quantification of different types of market available Chinese medicine extracts, pills and tablets. Results: The method allowed simultaneous determination of quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin in the concentration ranges of $0.00488-200{\mu}g/mL$, $0.625-320{\mu}g/mL$, $0.07813-320{\mu}g/mL$ and $0.03906-320{\mu}g/mL$, respectively. The limits of detection and quantification, respectively, were 0.00488 and $0.03906{\mu}g/mL$ for quercetin, 0.62500 and $2.50000{\mu}g/mL$ for bisdemethoxycurcumin, 0.07813 and $0.31250{\mu}g/mL$ for demethoxycurcumin, and 0.03906 and $0.07813{\mu}g/mL$ for curcumin. The percent relative intra day standard deviation (% RSD) values were $0.432-0.806{\mu}g/mL$, $0.576-0.723{\mu}g/mL$, $0.635-0.752{\mu}g/mL$ and $0.655-0.732{\mu}g/mL$ for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and those for intra day precision were $0.323-0.968{\mu}g/mL$, $0.805-0.854{\mu}g/mL$, $0.078-0.844{\mu}g/mL$ and $0.275-0.829{\mu}g/mL$, respectively. The intra day accuracies were 99.589%-100.821%, 98.588%-101.084%, 9.289%-100.88%, and 98.292%-101.022% for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and the inter day accuracy were 99.665%-103.06%, 97.669%-103.513%, 99.569%-103.617%, and 97.929%-103.606%, respectively. Conclusion: The method was found to be simple, accurate and precise and is recommended for routine quality control analysis of commercial Chinese medicine products containing the flour flavonoids as their principle components in the extracts.