• Journal of the Korean Society of Food Science and Nutrition
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• v.33 no.2
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• pp.381-385
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• 2004

This study was conducted to develop an HPLC method for determining pantothenic acid in fortified foods which has typically been determined by microbiological assay (MBA) according to AOAC and Korean Food Code approved methods. Pantothenic acid was determined by reversed-phase ion-pair HPLC using UV absorption (200 nm) after extraction with 20 mM potassium phosphate solution by sonication. The recovery of spiked samples and detection limit (LOD) by HPLC were 83.5∼109.6% and 0.5 ppm (mg/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of pantothenic acid analyzed in all tested samples (n=13) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 91.9∼117.6%. There was not significant difference (p<0.01) between the HPLC and MBA methods and the equation of the regression curve was y=1.1428x-0.2269 (r=0.9842). This proposed HPLC method for determining pantothenic acid appears to be suitable for determining pantothenic acid concentrations above 0.25 mg/100 g in fortified foods.

• Natural Product Sciences
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• v.10 no.1
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• pp.40-42
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• 2004

A simple quantitative HPLC method has been developed for differentiating two plants of Asteraceae family viz. S. costus and A. lappa by using a pharmacologically active constituent chlorogenic acid and symmetry C18 column clubbed with a binary gradient using acetonitrile: 0.1% phosphoric acid and detected using a PDA at 327 nm. Quantitatively chlorogenic acid was found to be more in A. lappa (0.140%) than in S. costus (0.087%).

• Journal of Food Hygiene and Safety
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• v.35 no.3
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• pp.213-218
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• 2020

This study was conducted to develop a method of analysis for 4-hydroxy-L-isoleucine in the seed extract of fenugreek (Trigonella foenum graecum), a health functional food that contains dietary fiber. The analytical method for 4-hydroxy-L-isoleucine was derived with O-phthaldialdehyde reagent (OPA) and determined by HPLC-PDA. The method was performed on a Capcell Pak C₁₈ UG 120 column (4.6×250 mm, 5 ㎛) in isocratic elution mode using disodium phosphate and acetonitrile. The validation of the developed analytical method was conducted by evaluating several parameters; selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy and repeatability. Excellent linearity (R²=0.999) was observed for 4-hydroxy-L-isoleucine in the concentration range (5-100 ㎍/mL). Observed recoveries of these compounds were found to be between 91.7 and 96.4%. Precision was between 0.2 and 2.4% relative standard deviation (%RSD).

• Journal of Food Hygiene and Safety
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• v.28 no.1
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• pp.19-23
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• 2013

A simple and rapid method has been developed and validated for simultaneous determination of each macrolides residues (spiramycin, josamycin, tilmicosin, tylosin) in chicken muscle by high-performance liquid chromatography- photo diode array (HPLC-PDA). Chicken muscle sample have been extracted with liquid-liquid extraction process; analytes was extracted by acetonitrile, and then defatted with hexane saturated by acetonitrile. The HPLC separation was performed on a Unison UK-$C_{18}$ ($150mm{\times}3.0mm$, $3{\mu}m$) with a gradient system of 0.1% trifloroacetic acid (TFA) and 0.1% trifloroacetic acid (TFA) in acetonitrile as the mobile phase. The drugs were detected at 232 nm for spiramycin and josamycin, and 287 nm for tilmicosin and tylosin. The limits of quantification (LOQs) were between 27 and $59{\mu}g/kg$; and the intra- and inter-day precision (relative standard deviation; RSD) was between 0.9-13.2 and 2.4-13.1%, respectively in chicken muscle sample. The method may has been successfully applied for multiresidue determination of four macrolides below the maximum residue limits (MRLs) established by the European Union (EU).

• Korean Journal of Pharmacognosy
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• v.48 no.4
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• pp.343-349
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• 2017

The current definition of Arismatis Rhizoma is the tuberous root of Alisma orientale Juzepzuk in the Korean Pharmacopoeia, but there is still no marker compound. So it has difficulties in quality control. Therefore, in this study, we have established a method to analyze alisol B and alisol B acetate using HPLC as a marker compounds of Arismatis Rhizoma. As the result of the analysis, alisol B content was ranged from 0.02% to 0.50% and alisol B acetate content was ranged from 0.12% to 0.25% in 40 samples. The stability of alisol B and alisol B acetate was investigated during 24 months. As a result, alisol B acetate was significantly decreased. The marker compound of Arismatis Rhizoma is alisol B acetate and the content of 0.05% or more is suitable by applying the stability results.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.143-148
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• 2022

This study was to investigate an analytical method for determining dieckol content in Ecklonia stolonifera extract. According to the guidelines of International Conference on Harmonization. Method validation was performed by measuring the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of dieckol using high-performance liquid chromatography-photodiode array. The results showed that the correlation coefficient of calibration curve (R²) for dieckol was 0.9997. The LOD and LOQ for dieckol were 0.18 and 0.56 ㎍/mL, respectively. The intra- and inter-day precision values of dieckol were approximately 1.58-4.39% and 1.37-4.64%, respectively. Moreover, intra- and inter-day accuracies of dieckol were approximately 96.91-102.33% and 98.41-105.71%, respectively. Thus, we successfully validated the analytical method for estimating dieckol content in E. stolonifera extract.

• Natural Product Sciences
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• v.26 no.4
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• pp.326-333
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• 2020

The aerial parts of Eclipta prostrata is used as a traditional medicine and vegetable. In traditional folk medicine, it is used for treatment of hemorrhages, hepatic, disease, renal injuries, hair loss, tooth mobility, and viper bites. In this study, ten compounds (1 - 10) were isolated from the aerial parts of E. prostrata. A reliable high performance liquid chromatography equipped with photometric diode array detector (HPLC-PDA) method was developed to simultaneously quantitate 10 marker compounds [chlorogenic acid (1), paratensein 7-O-��-ᴅ-glucoside (2), quercetin 7-O-��-ᴅ-glucoside (3), luteolin 7-O-��-ᴅ-glucoside (4), apigenin 7-O-��-ᴅ-glucoside (5), apigenin 4'-O-��-ᴅ-glucoside (6), apigenin (7), luteolin (8), wedelolactone (9), and paratensein (10)]. In addition, compounds 5 and 6 showed considerable inhibitory effects against protein-tyrosine phosphatase 1B (PTP1B) enzyme. Moreover, compounds 6 - 8, and 10 exhibited potent α-glucosidase inhibitory effects with IC50 values of 24.5 ± 1.9, 33.0 ± 0.5, 45.5 ± 0.1, and 23.8 ± 1.0 µM, respectively. All compounds (1 - 10) showed considerable acetylcholinesterase (AChE) inhibitory effects with IC50 ranging from 30.1 to 75.2 µM.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.52-57
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• 2019

Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column ($3{\times}150mm$, $3{\mu}m$) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9994 and the limit of detection and limit of quantitation were $0.011{\mu}g/mL$ and $0.033{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and $10{\mu}g/mL$ were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.

• Natural Product Sciences
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• v.21 no.1
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• pp.20-24
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• 2015

Cyanidin-3-glucoside (C3G) and cyanidin-3-rutinoside (C3R) were isolated by high-performance countercurrent chromatography (HPCCC) using a two-phase solvent system composed of tert-butyl methyl ether/n-butanol/acetonitrile/water/trifluoroacetic acid (1 : 3 : 1 : 5 : 0.01, v/v) to give pure C3G (34.1 mg) and C3R (14.3 mg) from 1.5 g crude mulberry fruit extract. Using the pure C3G and C3R, a reliable high-performance liquid chromatography (HPLC) method was developed and validated to determine the C3G and C3R contents in mulberry fruit. C3G and C3R were separated simultaneously using an Eclipse XDB-C18 column ($4.6{\times}250mm$ I.D., $5{\mu}m$) coupled with a photodiode array detector (PDA). The gradient elution of the mobile phase consisting of acetonitrile (0.5% formic acid) and water (0.5% formic acid) was applied (1.0 mL/min), and the detection wavelength was 520 nm. The calibration curves of C3G and C3R showed good linearity (both with $r^2=0.9996$) in the concentration range $15.625-500{\mu}g/mL$, and the relative standard deviations (RSD%) of intra- and inter-day variability were in the ranges 2.1 - 8.2% and 4.1 - 17.1%, respectively. The accuracies were ranged 96.5 - 102.6% for C3G and C3R, respectively. The developed HPLC method was used to determine the contents of C3G and C3R in newly harvested mulberry from eight different provinces of Korea.

• The Journal of Internal Korean Medicine
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• v.40 no.6
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• pp.1112-1121
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• 2019

Objectives: FDY003 is a raw material for medicine consisting of a natural product that is expected to have the advantages of low side effects and high efficacy. In this study, we predict the efficacy and the standardization of the drug by method validation of anticipated index compounds and the measurement of antioxidant activity. Methods: FDY003 is prepared by extracting and purifying 70% of ethyl alcohol (EtOH). The method validation of cordycepin and chlorogenic acid was determined by high-performance liquid chromatography-photo diode array (HPLC-PDA) and the content of FDY003 was calculated. In order to monitor the biological activity of FDY003, antioxidant activity was measured by 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2-azino bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), and ferric-reducing antioxidant power (FRAP). The equivalent values of antioxidants such as trolox, ascorbic acid, gallic acid, and caffeic acid were measured by ABTS and FRAP. Results: Chlorogenic acid and cordycepin were both found suitable for method validation in HPLC and FDY003 containing 9.92±0.50 and 17.97±0.27 ㎍/g, respectively. In DPPH, the electron donating ability (EDA) value of FDY003 was increased in a concentration dependent manner. FDY003 confirmed antioxidant activity by ABTS and FRAP. Conclusions: FDY003 contains certain components including cordycepin and chlorogenic acid and has antioxidant ability by various mechanisms. Therefore, it is expected that FDY003 is capable of various physiological activities including anti-cancer activity.