• Analytical Science and Technology
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• v.20 no.4
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• pp.323-330
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• 2007

A simple and rapid HPLC method with fluorescence detection(FLD) for quantitation of penciclovir in human plasma using a monolithic column was developed and validated. Penciclovir and ganciclovir(internal standard, I.S.) were separated on a Chromolith column RP-18e ($4.6{\times}100mm$) with a mobile phase consisting of a mixture of (A) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (3/97, pH 2.5) and (B) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (50/50, pH 2.5) at a flow gradient of $1.6{\sim}4.0mL/min$. The retention times of penciclovir and internal standard were less than 4.0 min. Calibration curve was linear ($R^2=0.9994$) over a concentration range of $0.1{\sim}5{\mu}g/mL$. Intra-day precision, accuracy and inter-day precision were 1.36~8.55 %, 92.8~100.0 % and 0.93~5.62 %, respectively with a limit of quantitation at $0.1{\mu}g/mL$. The present HPLC-FLD method is sensitive, precise and accurate. The method described herein has been successfully used for the bioequivalence study of a famciclovir formulation product after oral administration to healthy Korean volunteers.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.49 no.4
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• pp.291-298
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• 2023

In this study, a quantitative analysis method was developed using high-performance liquid chromatography (HPLC) to analyze the content of ceramide NP in lotion, cream, and cleanser formulations in cosmetics. The analysis was performed using a C18 column, and the mobile phase was set at a ratio of 70 : 30 for acetonitrile and methanol, the flow rate was set to 0.8 mL/min, and the column temperature was set to 20 ℃. The method was verified by analyzing specificity, linearity, limit of detection, limit of quantitation, accuracy, and precision in accordance with the ICH guidelines. As a result of validating the method, the linearity of the calibration curve was excellent (R² = 0.99984). The accuracy of the lotion, cream, and cleanser formulations was confirmed with a recovery rate ranging from 95.11% to 100.48%. The precision analysis showed a low relative standard deviation (RSD) of less than 0.26%. The limit of detection was 0.902 ㎍/mL, and the limit of quantitation was 2.733 ㎍/mL. Through this quantitative analysis method of ceramide NP applied in cosmetics, it is expected to assist in the quality control of products by enabling measurement even when it is difficult to separate the main peak due to the influence of interfering substances.

• Journal of Life Science
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• v.34 no.1
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• pp.59-67
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• 2024

LS-RUG-com preparation in a complex extract from mixture of three natural plants. Rubus crataegifolius/unriped, Gardenia jasminoides and Ulmus marcrocarpa that have been widely used in traditional functional health food. This study was conducted to establish the HPLC analysis methods that can be used to establish quantitative analysis of R. crataegifolius, G. jasminoides and U. macrocarpa for standardization of LS-RUG-com preparations. HPLC analysis methods for simultaneous determination of ellagic acid and geniposide and single determination of catechin-7-O-β-D-apiofuranoside were established for the quality control of natural plants complex (LS-RUG-com). Validation of HPLC analysis were performed by checking specificity, accuracy, precision, limit of detection and quantitation, and linearity following ICH (International Council for Harmonisation) guideline. As the result of quantitative analysis, the contents of ellagic acid, geniposide and catechin-7-O-β-D-apiofuranoside in each plant extracts were 11.2 mg/g (ellagic acid) and 72 mg/g (geniposide) and 10.2 mg/g (catechin-7-O-β-D-apiofuranoside). The contents of ellagic acid, geniposide and catechin-7-O-β-D-apiofuranoside in LS-RUG-com were 4.62~6.82 mg/g (ellagic acid), 19.2~28.8 mg/g (geniposide) and 1.36~2.04 mg/g (catechin-7-O-β-D-apiofuranoside) respectively.

• Korean Journal of Environmental Agriculture
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• v.24 no.1
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• pp.45-55
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• 2005

This study was undertaken to find out necessary measures to improve the tolerance setting system of pesticide residues on food crops in Korea which is scientifically reasonable and harmonizable with international standards. Information on tolerance setting systems of pesticide residues by Codex Alimentarius Commission, Joint FAO/WHO Meeting of Experts on Pesticide Residues, USA, EU, Japan and Taiwan was collected and analyzed. On the basis of information in the above countries, necessary actions to be taken by the Korean regulatory authorities were recommended with respect to priority setting, maximum residue limits (MRLs) setting based on field residue data, group MRLs, minor crop problems, quantitation limit and dietary intake assessment.

• Bulletin of the Korean Chemical Society
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• v.31 no.5
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• pp.1192-1198
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• 2010

Pharmaceuticals and personal care products (PPCPs) are emerging contaminants in the aquatic environment. Many pharmaceuticals are not completely removed during wastewater treatment, leading to their presence in wastewater treatment effluents, rivers, lakes, and ground water. Here, we developed analytical methods for monitoring ten pharmaceuticals from surface water by LC/ESI-MS/MS. For sample clean-up and extraction, MCX (mixed cation exchange) and HLB (hydrophilic-lipophilic balance) solid-phase extraction (SPE) cartridges were used. The limits of detection (LOD) in distilled water and the blank surface water were in the range of 0.006 - 0.65 and 1.66 - 45.05 pg/mL, respectively. The limits of quantitation (LOQ) for the distilled water and the blank surface water were in the range of 0.02 - 2.17 and 5.52 - 150.15 pg/mL, respectively. The absolute recoveries for fortified water samples were between 62.1% and 125.4%. Intra-day precision and accuracy for the blank surface water were 2.9% - 24.1% (R.S.D.) and -16.3% - 16.3% (bias), respectively. In surface wastewater near rivers, chlortetracycline and acetylsalicylic acid were detected frequently in the range of 0.017 - 5.404 and 0.029 - 0.269 ng/mL, respectively. Surface water near rivers had higher levels than surface water of domestic treatment plants.

• Bulletin of the Korean Chemical Society
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• v.33 no.2
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• pp.559-563
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• 2012

An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

• Analytical Science and Technology
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• v.30 no.3
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• pp.154-158
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• 2017

The Korean Pharmacopoeia (KP XI), British Pharmacopoeia (BP 2013) and Japanese Pharmacopoeia contain monographs for the quality control of raw fusidate sodium and its formulations using high performance liquid chromatography (HPLC). However, the assay method for the determination of fusidate sodium in commercial tablets is titration which is less specific than HPLC. In this study, we present an alternative HPLC method for quantitation of fusidate sodium in tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9999$), while the RSDs for intra- and inter-day precision were 0.25-0.37 % and 0.11-0.60 %, respectively. Accuracies ranged from 99.46-100.85 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

• Analytical Science and Technology
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• v.32 no.6
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• pp.217-224
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• 2019

In this study, to evaluate the effectiveness and safety of oral therapy using Gastrodiae Rhizoma, a new HPLC-PDA analysis method was developed for the simultaneous quantitation of the three major components: (1) gastrodin, (2) gastrodigenin, and (3) p-hydroxybenzaldehyde, in steam processed and unprocessed tubers of Gastrodia elata Blume. The clear separation of the three components was achieved on a C18 column (250 × 4.6 mm, 5 ㎛) by gradient elution using water (including 0.1 % formic acid) and acetonitrile as the mobile phase. The flow rate was 1.0 mL/min, and the UV detector wavelength was set at 270 nm. The results demonstrate satisfactory linearity, recovery, precision, accuracy, stability, and robustness. The established HPLC-PDA method was applied to quantify three major compounds in 59 samples of G. elata Blume tubers. Finally, the steam processed and unprocessed tubers of G. elata Blume were successfully distinguished by pattern recognition analysis.

• The Korean Journal of Physiology and Pharmacology
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• v.7 no.4
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• pp.247-250
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• 2003

A simple and sensitive assay method was developed for cefepime in human plasma using high performance liquid chromatography (HPLC). Cefepime and cefadroxil (the internal standard) were extracted from heparinized human plasma by simple deproteination with perchloric acid. The extract was injected into an Atlantis dC18 column ($250{\times}4.6$ mm; particle size $5{\mu}m$, Waters) and the column was eluted with methanol and 0.01 M dihydrogen phosphate at pH 3.0 (15：85 v：v) as a mobile phase at a flow rate of 0.7 mL/min. Linearity was confirmed for the range 0.25 to $200{\mu}L/mL$ and the limit of quantitation was $0.25{\mu}L/mL$. The retention times were 10.2 min and 13.4 min for cefepime and cefadroxil, respectively. This method was successfully applied to a pharmacokinetic study of cefepime in plasma from bone marrow transplant patients.

• Journal of Environmental Health Sciences
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• v.32 no.1 s.88
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• pp.67-70
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• 2006

A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.