• Korean Journal of Pharmacognosy
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• v.40 no.2
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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.

• Korean Journal of Pharmacognosy
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• v.39 no.4
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• pp.316-323
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• 2008

In this study, we have investigated the HPLC analysis methods and quantitative analysis of standard compounds for quality standardization of a medicinal crude drug GCSB-5, a herbal formulation consisting of 6 medicinal plants (Acanthopanacis Cortex, Achyranthis Radix, Ledebouriellae Radix, Cibotii Rhizoma, Glycine Semen, Eucommiae Cortex) which are used in traditional medicine to treat various bone disorders. HPLC analysis methods of acanthoside D(Acanthopanacis Cortex), 20-hydroxyecdysone(Achyranthis Radix) which were known standard compounds among 6 medicinal plants were developed on crude material and product. 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. Content of acanthoside D and 20-hydroxyecdysone on raw material of GCSB-5 were decided at 0.577-0.578 mg/g and 0.311-0.312 mg/g. And we confirmed that content of acanthoside D and 20-hydroxyecdysone on GCSB-5 preparation were 0.302-0.303 mg/capsule and 0.113-0.115 mg/capsule.

• Korean Journal of Pharmacognosy
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• v.40 no.1
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• pp.18-24
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• 2009

GCSB-5 preparation is a purified extract from a mixture six herbal medicines (Acanthopanacis Cortex, Achyranthis Radix, Saposhnikoviae Radix, Cibotii Rhizoma, Glycine Semen Nigra, Eucommiae Cortex) that have been widely used in traditional medicine to treat various bone disorders. This study was carried out to obtain the HPLC analysis method that can be used to establish quantitative analysis of Glycine Semen Nigra and Eucommiae Cortex for standardization of GCSB-5 preparation. HPLC analysis methods for the simultaneous determination of genistin (Glycine Semen Nigra) and geniposide (Eucommiae Cortex) were established for the quality control of herbal medicinal 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. As the result of quantitative analysis, the contents of genistin and geniposide in the raw material of GCSB-5 preparation were 0.0426-0.0427 mg/g and 0.431-0.432 mg/g. And GCSB-5 preparation contained genistin of 0.0202-0.0203 mg/capsule and geniposide of 0.211-0.212 mg/capsule, respectively.

• Korean Journal of Pharmacognosy
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• v.41 no.1
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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.

• Journal of Soil and Groundwater Environment
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• v.14 no.6
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• pp.35-44
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• 2009

Naphthalene and TNT (2,4,6-trinitrotoluene) are defined by U.S. EPA as possible carcinogenic compounds known to have detrimental effects on the aquatic ecosystem and human body. There are, however, few researches on methods of analyzing micro-levels of naphthalene and TNT dissolved in groundwater. This study introduces and evaluates the newly developed analytical methods of measuring naphthalene and TNT in groundwater by using HPLC-FLD (Fluorescence detector) and MSD (Mass detector). The MDL, LOQ and salt effect of these methods, respectively, are compared with those of conventional methods which use HPLC-UV. For the analysis of naphthalene, HPLC-FLD was set in the maxima wavelength (Ex: 270 nM, Em: 330 nM) obtained from 3D-Fluorescence to be compared with HPLC-UV in 266 nM wavelength. The MDL ($0.3\;{\mu}g/L$) and LOQ ($2.0\;{\mu}g/L$) of naphthalene by using HPLC-FLD were approximately 80 times lower than those analyzed by HPLC-UV (MDL: $23.3\;{\mu}g/L$, LOQ: $163.1\;{\mu}g/L$). HPLC-MSD were used in comparison with HPLC-UV in 230 and 254 nM wavelength for the analysis of TNT. The MDL ($0.13\;{\mu}g/L$) and LOQ ($0.88\;{\mu}g/L$) of TNT analyzed by using HPLC-MSD were approximately 130 times lower than those obtained by using HPLC-UV in 230 nM (MDL: $16.8\;{\mu}g/L$, LOQ: $117.5\;{\mu}g/L$). The chromatogram of TNT analyzed by using HPLC-UV in 230 nM displayed elevated baseline as the concentration of ${NO_3}^-$ increases beyond 21 mg/L, while the analysis using HPLC-MSD did not demonstrate any change in baseline in presence of ${NO_3}^-$ of 63.7 mg/L which is 3.5 times higher than average concentration in groundwater. In conclusion, HPLC-FLD and HPLC-MSD may be used as suitable methods for the analysis of naphthalene and TNT in groundwater and drinking water. These methods can be applied to the monitoring of naphthalene and TNT concentration in groundwater or drinking water.

• Bulletin of the Korean Chemical Society
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• v.28 no.7
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• pp.1187-1194
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• 2007

The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. 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 three major isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

• Archives of Pharmacal Research
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• v.17 no.5
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• pp.337-342
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• 1994

Carbohydrate analysis is important in studying structure and activity of complex polysaccharides. New analytical method was applied to get an information on the composition of polysaccharides showing antitumor activity. Monosaccharides were labeled with 7-amino-1, 3-naph-thalenedisulfonic acid (7-AGA) by reductive amination and separated by HPLC. Five kinds of polysaccharides from Basidiomycetes were hydrolyzed and analyzed in combination with electrophresis and HPLC. At the same time, alditol acetate derivatives were prepared and analyzed by gas chromatography. Two different techniques using different derivatization methods showed very similar results. The monosaccharides from Coriolus versicolor and Cordyceps militaris were glucose and galactose. Phellinus linteus composed of glucose, glactose, mannose, arabinose and fucose. The HPLC method with fluorescence detector was very sensitive compared to other methods.

• Korean journal of food and cookery science
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• v.23 no.1 s.97
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• pp.150-155
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• 2007

This work was conducted to obtain a rapid, accurate, and precise procedure for free amino acids analysis in Doenjang with HPLC-OPA (high performance liquid chromatography using-phthalaldehyde) and AAA (automatic amino acid analyzer) methods. Different sample extraction procedures among water, 0.1 M perchloric acid, and 0.1% meta-phosphoric acid were also compared. The optimal extraction solvent was 0.1% meta-phosphoric acid for both the HPLC-OPA and AAA methods. Good recoveries for glycine and methionine were observed using the 0.1% meta-phosphoric acid extraction with HPLC-OPA method. Method precisions (% relative standard deviation) for the free amino acids ranged for 1.62% to 8.27%, in which the HPLC-OPA method with water extraction showed the lowest value at 1.62%. Inhibition rates of the free amino acids in Doenjang were greatest with an addition of NaCI at a 1% concentration.

• YAKHAK HOEJI
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• v.57 no.5
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• pp.362-368
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• 2013

High performance liquid chromatograph (HPLC) is the most frequently used analytical instrument in analytical laboratories for pharmaceutical analysis. In order to provide a high level of assurance for reliable data generated from the HPLC analysis, the performance qualification of the HPLC system is required. For this purpose, the performance of HPLC system should be regularly monitored by examining the key functions of the typical HPLC system (solvent delivery system, injector system, column oven, UV-VIS detector system). We have investigated the validation guidelines of the performance verification of these key modules for HPLC system. And we proposed and evaluated its validation guidelines and the related verification methods for pharmaceutical analysis that could be practically applied in Korea.

• Korean Journal of Environmental Agriculture
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• v.23 no.4
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• pp.251-257
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• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.