• YAKHAK HOEJI
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• v.55 no.1
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• pp.64-68
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• 2011

In this study, a high performance liquid chromatography-diode array detector method was established, for simultaneous determination of three compounds, berberine, palmatine and geniposide in Hwangryunhaedok-tang, To develop and validate method, $C_{18}$ column (5 ${\mu}M$, 4.6 mm${\times}$250 mm) was used with gradient mobile phase, water containing 0.1% trifluoroacetic acid (TFA) and MeOH at the column temperature of $30^{\circ}C$. UV wavelength was set at 230 and 280 nm. Validation of the chromatography method was evaluated by linearity, precision and accuracy test. Calibration curve of standard components showed good linearity ($R^2$ > 0.9999). The limits of detection (LOD) and limits of quantification (LOQ) varied from 0.05 to 0.17 ${\mu}g/ml$ and 0.15 to 0.53 ${\mu}g/ml$, respectively. The relative standard deviations (RSDs) data of intra-day and inter-day test were in less than 2.99% and 1.90%, respectively. The results of the accuracy test were in the range of 98.36 to 102.52% with RSDs values 0.32 to 1.98%. The results of validation indicated that this method was a very accurate and sensitive assay.

• Journal of Ginseng Research
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• v.40 no.4
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• pp.382-394
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• 2016

Background: Ginsenosides are the characteristic and principal components which manifest a variety of the biological and pharmacological activities of the roots and rhizomes of Panax ginseng (GRR). This study was carried out to qualitatively and quantitatively determine the ginsenosides in the cultivated and forest GRR. Methods: A rapid and sensitive ultra-high-performance liquid chromatography coupled with diode-array detector and quadrupole/time of flight tandem mass spectrometry (UPLC-DAD-QTOF-MS/MS) was applied to the qualitative analysis of ginsenosides and a 4000 QTRAP triple quadrupole tandem mass spectrometer (HPLC-ESI-MS) was applied to quantitative analysis of 19 ginsenosides. Results: In the qualitative analysis, all ingredients were separated in 10 min. A total of 131 ginsenosides were detected in cultivated and forest GRR. The method for the quantitative determination was validated for linearity, precision, and limits of detection and quantification. 19 representative ginsenosides were quantitated. The total content of all 19 ginsenosides in the forest GRR were much higher than those in the cultivated GRR, and were increased with the growing ages. Conclusion: This newly developed analysis method could be applied to the quality assessment of GRR as well as the distinction between cultivated and forest GRR.

• Korean Journal of Medicinal Crop Science
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• v.24 no.3
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• pp.237-245
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• 2016

Background: Cyanazine is used as a pre-emergent herbicide once during the growing season to control weeds of many upland crops worldwide. This study aimed to establish a method to determined cyanazine residue levels in major medicinal crops by using high performance liquid chromatography-UV detection/mass spectometry (HPLC-UVD/MS). Methods and Results: Cyanazine residue was extracted with acetone from the raw products of four representative medicinal plants - Scutellaria baicalensis, Paeonia lactiflora, Platycodon grandiflorum and Angelica gigas. The extract was diluted with a large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. It was then purifined using optimized Florisil column chromatography. HPLC analysis conducted using an octadecylsilyl column allowed the successful separation of cyanazine from co-extractives of the samples, and the amount was sensitively quantified by ultraviolet absorption at 225 nm with no interference. The accuracy and precision of the proposed method were validated by conducting recovery experiments on each medicinal crop sample fortified with cyanazine at two concentration levels per crop in triplicate. Conclusions: The mean recoveries ranged from 91.2% to 105.3% for the four representative medicinal crops. The coefficients of variation were less than 10%, irrespective of the sample types and fortification levels. The limit of quantification of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method was performed by liquid chromatography/MS using selected-ion monitoring technique to clearly identify the suspected residue.

• Journal of the Korean Applied Science and Technology
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• v.10 no.2
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• pp.11-18
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• 1993

Contents of vitamin $D_3$ and 25-OH-vitamin $D_3$ in marine animal products(20 species) were determined by HPLC. The isomers of vitamin D, $D_2$ and $D_3$, were not clearly separated on a reversed phase, ${\mu}$ Bonda Pak, with 20% methanol-acetonitrile, and on a normal phase, Zorbax SIL. with 0.4% isopropanol-hexane, but 25-OH-vitamin $D_2$ and-$D_3$ were separated on either ${\mu}$ Bonda Pak with 10% methanol-acetonitrile, or on Zorbax SIL with 2.2% isopropanol-hexane, respectively. Although levels of vitamin $D_3$ and 25-OH-vitamin $D_3$ varied remarkably according to species, their average value(fish : $l,l87{sim}36,007$ I.U/sample 100g, mussel : $58{\sim}1,706$ I.U/sample 100g, pickle: $1,208{\sim}79,358$ I.U/sample 100g) was greatly higher than that of meat($80{\sim}100$ I.U/sample 100g) and dairy products($400{\sim}800$ I.U/sample 100g). Fatty tissues of fish and pickled fish intestines contained high level of vitamin $D_3$ and 25-OH-vitamin $D_3$, while the clam and mussel known to have various kinds of sterol including ${\Delta}^7$-sterol showed very low levels of vitamin $D_3$ and its derivative.

• Archives of Pharmacal Research
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• v.19 no.6
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• pp.554-558
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• 1996

High-performance liquid chromatographic method was developed for the determination or LB 20304 (compound 1) in the plasma of rats and dogs. The analyte was deproteinized with 1 volume of methanol and 1/2 volume of 10% zinc sulfate, and the supernatant was injected onto a reversed-phase HPLC column. The mobile phase was a mixture of 24 parts of acetonitrile and 76 parts of 0.1% trifluoroacetic acid. The flow rate was 1 ml/min, and the effluent was monitored by fluorescence detector at an excitation wavelength of 337 nm and an emission wavelength of 460 nm. The retention time of compound 1 was 6.3 min. The assay of compound 1 was linear over the concentration range of 0.2-100.mu.g/ml in the plasma of rats and dogs. The lower limit of quantification was 0.2.mu.g/ml using 100.mu.l of plasma with a 97-99% accuracy and a 12-14% precision. In the 0.5, 5, and 50.mu.g/ml quality control samples, the intra- and inter-day accuracy were 88-95% and 88-97%, whereas intra- and interday precision were 0.5-6.6% and 0.2-9.3%, respectively, in the plasma of rats and dogs. The recoveries were 68-71% independent of concentration and species in the plasma. No interferences from endogenous substances were observed. Taken together, the above HPLC assay method by deproteinization and fluorescence detection was suitable for the determination of compound 1 in the preclinical pharmacokinetics.

• Korean Journal of Veterinary Service
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• v.43 no.4
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• pp.261-265
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• 2020

Each commercial cyromazine insecticide has different HPLC conditions. The aim of this study was to establish a standardized chromatographic method for the determination of cyromazine in commercial insecticides. The separation was achieved on two C18 columns - Waters® Bondapak C (4×300 nm i.d., 10 ㎛) and X bridge (4.6×250 nm i.d., 5 ㎛) using a mobile phase composed of water/methanol/ethanolamine (76:24:0.1, v/v), with UV detection at wavelengths 230 nm and 254 nm. A total of six commercial cyromazine insecticides were analyzed. In this study, the optimal high-performance liquid chromatography conditions for the analysis of cyromazine were as follows: a mobile phase of water/methanol/ethanolamine (76:24:0.1, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm using a X bridge C18 column (4.6×250 nm i.d., 5 ㎛) at a column temperature of 25℃. The calibration curve was linear in the concentration range of 5~50 ㎍/mL, with a correlation coefficient of 0.99995. The cyromazine detection limit was 0.2 ㎍/mL, and the limit of quantification was 0.59 ㎍/mL. The percentage recovery ranged from 99.8% to 101.0% for cyromazine, and the relative standard deviation was not over 2.0%. The cyromazine concentration ranged from 92.7% to 109.4% and was within the acceptable range (90~120%) for the percent of the labeled amount. This method was found to be suitable for determining cyromazine in commercial insecticides.

• Korean Journal of Pharmacognosy
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• v.51 no.4
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• pp.291-296
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• 2020

Filipendula glaberrima (FG) is a plant endemic to South Korea. It is economically important as a food source and used as a medicine in treating ailments. Filipendula flowers are characterized by the presence of several polyphenolic constituents. The aim of this study is to determine the content of (+)-catechin in Filipendula glaberrima collected from different regions at different flowering stages. High-performance liquid chromatography with a gradient elution system (0.5% acetic acid in water : acetonitrile = 95 : 5 to 0 : 100 for 35 min) was used. A reverse-phase INNO column with UV detection at 278 nm was employed. The results revealed that F. glaberrima from Mt. Odae has the highest (+)-catechin content (10.600 mg/g). Furthermore, its content was the lowest in samples collected during the pre-flowering period and the highest at the early-flowering stage. This study provides a basis in establishing the optimal period and the best region for collecting F. glaberrima with maximized (+)-catechin yield.

• Fashion & Textile Research Journal
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• v.23 no.6
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• pp.844-851
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• 2021

Due to the increase in consumers' interest about well-being, interest in eco-friendly products has been increasing due to the harmful effects of various harmful substances contained in textile products and environmental issues. As a result, natural dyes of less potential risk than synthetic dyes and digital textile printing(DTP) textile products with less environmental pollution are drawing attention. However, due to the lack of evaluation criteria for DTP textile products with natural ink and the nature of many colors are stacked layer by layer for dying, the need for simultaneous analysis is emerging. To evaluate whether the natural dye is derived from natural ingredients, the biocarbon content is analyzed. However, in the case of ink made using natural dyes and DTP textile products using natural ink, it is difficult to analyze the biocarbon content due to the limitation of the presence of a small amount of dye contained therein. In this study, we were shown the possibility of natural derived verification by cross-checking the analytes of natural dyes (Persicaria tinctoria, an indigo dye; Dactylopius coccus, a light red; and Curcum longa L., i.e., turmeric) and natural ink with HPLC-MS/MS. The coefficient of determination was 0.999 or higher, the limit of quantification was 0.647-3.664 ㎍/L and a %RSD of each indicator material was less than 10. Then, the extraction amount of natural dyes for five patterned fabrics was analyzed.

• The Korea Journal of Herbology
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• v.29 no.1
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• pp.13-18
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• 2014

Objectives : Iridoid glycoside, swertiamarin is a well known bioactive component found in Swertia japonica Makino (SJ). In this study, we tried to optimize a suitable method which would extract swertiamarin effectively. Methods : Extraction of SJ was carried out by various conditions of time (5 - 60 min), temperature ($30-70^{\circ}C$), solvent (from non-polar to polar), and ratio of solvnet / sample (10 : 1 - 40 : 1) using ultrasonic extractor. Swertiamarin in SJ extracts was quantified by high performance liquid chromatography - Phtodiode array detector (HPLC-PDA) using C18 column and the analytical procedure was validated by evaluation of specificity, range, linearity, accuracy (recovery), precision (intra- and inter day variability), limit of detection (LOD), and limit of quantification (LOQ). Results : An efficient extraction condition for swertiamarin in SJ was optimized using sonicator extraction (temperature $40^{\circ}C$, solvent 20% methanol, solvent / sample (20 : 1), and time 10 min. Analytical procedure was optimized by HPLC-PDA using isocratic solvent system of acetonitrile and water (9 : 91), and the method was validated in regard to linearity (correlation coefficient, $R^2$ > 0.9999), range ($50-1000{\mu}g/mL$), intra- and inter-precision (RSD < 5.0 %), and recovery (99 -103 %). LOD and LOQ were 0.051 and $0.155{\mu}g/mL$, respectively. Conclusion : An optimized method of extraction for swertiamarin in SJ was established through conditions of diverse extraction and the validation result indicated that the method is suited for the determination of swertiamarin in SJ.

• Analytical Science and Technology
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• v.36 no.4
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• pp.180-190
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• 2023

The presence of process related impurities in any drug or the drug product was associated with its safety, stability and efficacy. The overall literature survey proved that there is no method published on the assessment of process related impurities in brigatinib. In this study, a simple, reliable and stable HPLC qualitative method was reported for quantification of process related impurities with easy and quick extraction procedure. The impurities along with standard brigatinib was resolved on Lichrospher^® C18 (250 mm × 4.6 mm; 5 ㎛ particle size) column in room temperature using methanol, acetonitrile, pH 4.5 phosphate buffer in 55:25:20 (v/v) at 1.0 mL/min as mobile phase and UV detection at 261 nm. The method produces well resolved peaks at retention time of 4.60 min, 12.28 min, 3.37 min, 7.34 min and 8.39 min respectively for brigatinib, impurity A, B, C and D. The method produces a very sensitive detection limit of 0.0065 ㎍/mL, 0.0068 ㎍/mL, 0.0053 ㎍/mL and 0.0058 ㎍/mL for impurity A, B, C and D respectively with calibration curve linear in the concentration range of 22.5-135 ㎍/mL for brigatinib and 0.0225-0.135 ㎍/mL for impurities. The method produces all the validation parameters under the acceptable level and doesn't produces any considerable changes in peak area response while minor changes in the developed method conditions. The method can effectively resolve the unknown stress degradation products along with known impurities with less % degradation. The method can efficiently resolve and quantify the impurities in formulation and hence can suitable for the routine quality analysis of brigatinib in raw material and formulation.