• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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• pp.244.1-244.1
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• 2003

We aimed at determining bioavailability of clonazepam, an anxiolytic drug, and developing a simple analysis in human blood using HPLC. A rapid and sensitive HPLC method was developed and validated using reverse-phase C18 column with retension time and limit of quantification of clonazepam being 2.58 min and 5hg/ml, respectively. Quantification was performed at 235 nm with p-hydroxybenzoic acid ethyl ester as internal standard. The method involved a simple extraction. In order to study blood level profile in time, sight volunteers were enrolled and orally took 6 mg clonazepam once. (omitted)

• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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• pp.240.2-240.2
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• 2003

We aimed at determining bioavailability of procainarnide HCl, an antiarrhythmic drug, and developing a simple analysis in human blood using HPLC. A rapid and sensitive HPLC method was developed and validated using reverse-phase C18 column with retension time and limit of quantification of procainamide HCl being 2.58 min and 50ng/ml, respectively. Quantification was performed at 275 nm with caffeine as internal standard. The method involved a simple extraction. In order to study blood level profile in time, eight volunteers were enrolled and orally took 250 mg procainamide HCl once. (omitted)

• Bulletin of the Korean Chemical Society
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• 제35권3호
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• pp.765-769
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• 2014

An analytical methodology was developed for qualitative and quantitative impurity profiling of the coloring agent Sudan III by high-performance liquid chromatography (HPLC)-diode array detection (DAD). The impurities in commercial Sudan III were characterized by comparison of their retention times and UV spectra with those of authentic standards. Four impurities regulated by International Committees in Sudan III were quantified by HPLC-selective UV detection. The impurities in Sudan dye were successfully separated on a reversed phase C18-column within 25 min and sensitively detected by UV spectrometry at two selective wavelengths. Method validation was conducted to determine linearity, precision, accuracy, and limit of quantification (LOQ). The linear dynamic range extended from 0.002 to 4.0%, with a correlation coefficient (R2) greater than 0.995. The LOQs of the impurities ranged from 8.04 to $54.29{\mu}g/mg$. Based on the established method, the levels of regulated impurities in five commercial Sudan III dyes were determined.

• 분석과학
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• 제34권4호
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• pp.153-159
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• 2021

In this study, we describe the development of a new high-performance liquid chromatography (HPLC) method for the simultaneous analysis of six bioactive compounds (including gallic acid, epicatechin 3-gallate, quercitrin, afzelin, quercetin, and kaempferol) from Orostachys japonicus. The extraction method was investigated and optimization of the extraction time (min), solvent composition (%), and solvent to material ratio were conducted. As a result, 30 min extraction with 50% methanol and 40:1 mL/g of solvent: material ratio achieved the highest extraction efficiency with a yield of 3.32 mg/g. Furthermore, the developed HPLC method was validated and the correlation coefficient (R) values were within the satisfactory range of 0.9995-0.9999 over the linearity range of 1.53-417 ㎍/mL. The limit of detection and limit of quantification for the six active components were between 0.03-0.08 ㎍/mL and 0.08-0.26 ㎍/mL, respectively. With these newly optimized and developed methods, four batches of O. japonicus were analyzed to confirm the high extraction efficiency of the method and the feasibility of an application.

• Natural Product Sciences
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• 제14권3호
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• pp.147-151
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• 2008

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, baicalin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Eul-Ja-Tang (EJT). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/VIS detector (DAD) was used for the detection and the wavelength for quantification was set at 250 nm. The presence of baicalin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. Both baicalin and glycyrrhizin showed good linearity ($r^2$ > 0.999) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 5% and the limits of detection (LOD) were about 30 ng. The mean recovery of each compound was 99.5 - 101.2% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of baicalin and glycyrrhizin in three commercial products of EJT, which resulted in the difference in the contents of these compounds. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial EJT products.

• Journal of Pharmaceutical Investigation
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• 제39권1호
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• pp.23-27
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• 2009

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, paeoniflorin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Sayuk-san (SYS). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, $4.6mm\;I.D.{\times}150mm$) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/vis detector (DAD) was used for the detection and the wavelength for quantification was set at 230 nm. The presence of paeoniflorin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. All two compounds showed good linearity ($r^2$>0.996) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 7.3% and the limits of detection (LOD) were less than 55.7 ng. The mean recovery of each compound was $102.3{\sim}111.1%$ with R.S.D. values less than 4.6%. This method was successfully applied to the determination of contents of paeoniflorin and glycyrrhizin in three commercial products of SYS. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial SYS products.

• Journal of Ginseng Research
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• 제45권2호
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• pp.246-253
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• 2021

Background: Ginseng is one of the most valuable herbal supplements. It is challenging to perform quality control of ginseng products due to the diversity of bioactive saponins in their composition. Acid or alkaline hydrolysis is often used for the structural elucidation of these saponins and sugars in their side chains. Complete transformation of the original ginsenosides into their aglycones during the hydrolysis is one of the ways to determine a total saponin group content. The main hurdle of this approach is the formation of various by-products that was reported by many authors. Methods: Separate HPLC assessment of the total protopanaxadiol, protopanaxatriol and ocotillol ginsenoside contents is a viable alternative to the determination of characteristic biomarkers of these saponin groups, such as ginsenoside Rf and pseudoginsenoside F₁₁, which are commonly used for authentication of P. ginseng Meyer and P. quinquefolius L. samples respectively. Moreover, total ginsenoside content is an ideal aggregated parameter for standardization and quality control of ginseng-based medicines, because it can be directly applied for saponin dosage calculation. Results: Different hydrolysis conditions were tested to develop accurate quantification method for the elucidation of total ginsenoside contents in herbal products. Linearity, limits of quantification, limits of detection, accuracy and precision were evaluated for the developed HPLC-MS method. Conclusion: Alkaline hydrolysis results in fewer by-products than sugar elimination in acidic conditions. An equimolar response, as a key parameter for quantification, was established for several major ginsenosides. The developed approach has shown acceptable results in the analysis of several different herbal products.

• 한국동물위생학회지
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• 제23권2호
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• pp.137-142
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• 2000

In order to develop a good separation and simultaneous analysis of different sugar in an artificial mixed sugar solution, we analyzed 10 sugar components in an artificial mixed sugar solution composed of fructose, glucose, mannitol, sucrose, maltose, lactose, xylose, xylitol erythritol, and trehalose with using HPLC-ELSD or HPLC-RI. Separation and quantification by HPLC-ELSD was superior to those by HPLC-RI and detection sensitivity by HPLC-ELSD was higher then that by HPLC-RI as micorgram($\mu\textrm{g}$) level. 1. The units of minimal detectable limits were showed $\mu\textrm{g}$/$m\ell$ and ng/$m\ell$ by the HPLC-RI and HPLC-ELSD, respectively. 2. The condition of ELSD was drift tube temperature $82^{\circ}C$, $N_2$ gas flow rate 2.10 SLPM, and colum oven temperature $30^{\circ}C$, respectively. Isolation and recovery rates of single sugar from the multiple sugar solution was higher at the condition (time: flow rate: D.W.:ACN MeOH, min : $m\ell$/min:v:v:v) of linear gradient elution of mobile phase as 0 : 1.00 : 15 : 85 : 0.1 : 1.00 : 6 : 90 : 4, 17 : 1.00 : 10 : 70 : 20, 28 : 1.00 : 15 : 85 : 0 an 35 : 1.00 : 15 : 85 : 0, in order.

• Journal of Applied Biological Chemistry
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• 제64권3호
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• pp.285-290
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• 2021

Salicornia herbacea is a type of salt marsh plant that has been used in traditional medicine to treat several diseases. Isorhamnetin-3-O-glucoside (I3G) and quercetin-3-O-glucoside (Q3G) are major flavonoids in S. herbacea that are known to exert various pharmacological activities. Therefore, our study sought to validate and optimize an HPLC/UV-based analytical method for I3G and Q3G yield quantification, as well as to determine its limit of detection, limit of quantification, linearity, precision, and accuracy. Upon testing a concentration range of 31.5-1.9 ㎍/mL the results exhibited good linearity (r² ≥0.9996 and r² ≥0.9999 for I3G and Q3G, respectively), and the procedure was deemed precise (relative standard deviation of ≤3.19 and ≤3.85%, respectively), and accurate (102.6-105.0 and 92.9-95.2%, respectively). The results showed that our proposed method could be used for rapid I3G and Q3G evaluation in S. herbacea.

• Natural Product Sciences
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• 제12권1호
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• pp.55-61
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• 2006

A description of simple, isocratic and precise reversed phase HPLC methods is given for simultaneous quantification of pholcodine and ephedrine hydrochloride together with either carbinoxamine maleate or terfenadine in antitussive-antihistaminic oral pharmaceutical formulations. Separations were carried out on X-Terra and symmetry shield C18 column $(250\;{\times}\;4.6\;mm,\;5\;{\mu}m)$. The used isocratic elution systems were either $0.02\;M\;KH_2PO_4-acetonitrile$ in the ratio of 75 : 25 and pH adjusted to 7.70 with orthophosphoric acid or sodium hydroxide, for syrup (method A), or 0.02 octanesulphonic acid sodium salt solution-acetonitrile-acetic acid in the ratio of 75 : 25 : 0.5 for suspension (method B). The elution of both mixtures was achieved with a flow rate of 1 ml/min. Detection was carried out by UV absorbance at wavelengths of 220 and 250 nm for syrup and suspension, respectively. The quantification of the components in synthetic mixtures and actual syrup and suspension were calculated using the internal standard technique with metoclopramide HCl and codeine phosphate as internal standards (IS), respectively. The methods, for both mixtures, were validated and met all the requirements for the quality control analysis recommended by FDA and ICH.