• Journal of Applied Biological Chemistry
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• v.65 no.4
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• pp.343-348
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• 2022

This study was performed to establish an analytical method for the standardization of Angelicae Dahuricae Radix as a functional ingredient. We established six compounds including oxypeucedanin hydrate (1), byakangelcol (2), oxypeucedanin (3), imperatorin (4), phellopterin (5) and isoimperatorin (6) as marker compounds of Angelicae Dahuricae Radix. An analytical method using Ultra Performance Liquid Chromatography (UPLC) was established and validated for marker compounds of Angelicae Dahuricae Radix. The specificity was confirmed by the chromatogram from UPLC and the value of coefficient determination was also higher than 0.999, indicating high linearity. The relative standard deviation (RSD) and recovery of marker compounds were less than 5% and in the range of 90- 110%, respectively, which means that this method has high accuracy and precision. Therefore, this analytical method could be used as basic data for the development of functional ingredients for health functional food of Angelicae Dahuricae Radix.

• Analytical Science and Technology
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• v.36 no.3
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• pp.105-112
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• 2023

Lycopene, a carotenoid hydrocarbon is known to have effects on reducing cardiovascular risk factors, blood lipids, and blood pressure. Thus, a lot of supplementary foods with lycopene in several dosage forms like soft capsule filled with liquid and hard capsule filled with powder are available in a market. Recently, however, our research group found that the lycopene assay in Supplementary Food Code of South Korea is only valid for oily lycopene preparation. Thus, here, we developed a simple method to determine lycopene in solid preparations for Supplementary Food Code of South Korea using saponification and liquid chromatography with an absorbance detector. The method was validated following Ministry of Food and Drug Safety guidelines. All validation parameters observed in this study were within acceptable criteria of the guidelines (selectivity, linearity of r² ≥ 0.991, lower limit of quantification of 0.0149 mg/mL, accuracy as recovery (R) between 92.70 and 97.18 %, repeatability as relative standard deviation (RSD) values of R between 0.85 and 1.59 %, and reproducibility as the RSD value of interlaboratory R of 3.70 %). Additionally, the practical sample applicability of the validated method was confirmed by accuracy between 98.81 and 101.59 % observed from its lycopene certified reference material (CRM) analyses. Therefore, the present method could contribute to fortify the supplementary food safety management system in South Korea.

• Analytical Science and Technology
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• v.37 no.3
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• pp.143-154
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• 2024

In this study, we improved the vitamin C test method and reviewed data on the adjustable range of chromatography conditions for quantification. First, we adjusted the mobile phase conditions such as solvent composition, salt concentration, pH and column temperature and in particular, it was confirmed through an improved test method that the peak derived from the buffer solution could be clearly separated from the target component, vitamin C by adjusting the pH. The retention time of vitamin C was partially changed by adjusting the column diameter, length and particle size but the number of theoretical plates indicated similar values and did not affect the separation and quantitative analysis of the target component. The flow rate according to the column specifications was derived from the equation proposed by the U.S. FDA (Food and Drug administration) and the Korean MFDS (Ministry of Food and Drug Safety), and evaluation of the applicability to vitamin complexes showed high selectivity for vitamin C even with altered stationary phase conditions and flow rates. In conclusion, vitamin C can be optimally separated and detected by changing the chromatographic method conditions and it was confirmed that the mobile and stationary phase conditions of liquid chromatography can be slightly adjusted in case the assay method uses an isocratic elution.

• Analytical Science and Technology
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• v.24 no.5
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• pp.345-351
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• 2011

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.33 no.4
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• pp.263-267
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• 2007

Parabens are used in nearly all types of cosmetics and toiletries because they are formulated well and have broad spectrum of activity, interness, low costs and excellent chemical stability in relation to pH. 2-phenoxyethanol and chlorphenesin are common preservatives which are usually used in combination with parabens in cosmetics. Toxicity of parabens is generally low but application of parabens to damaged or broken skin has resulted in sensitization. Moreover, the possibility of their estrogenic potential, anesthetic effects and reproductive toxicity has been reported. Consequently there are some regulations in use of parabens. And the maximum permitted concentrations of chlorphenesin and 2-phenoxyethanol in cosmetic products are authorized by the same reasons. So it is important to control and estimate the amount of parabens in products. In this article, we proposed a valid method for the simultaneous determination of 8 preservatives including parabens in a short time using ultra performance liquid $chromatography^{TM}\;(UPLC^{TM})$. Separation of eight components was achieved in less than 10 min and resolutions were reasonable (USP resolution ${\geqq}\;2$). And limit of detection and quantification were evaluated. The method was suitably validated for specificity, linearity, precision (repeatability, intermediate precision) and accuracy for assay (recovery) based on International conference on harmonisation (ICH) guideline. The method was applicable to analysis of preservatives in cosmetic products.

• Journal of the Korean Society of Food Science and Nutrition
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• v.41 no.11
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• pp.1554-1558
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• 2012

Method development and validation of ellagic acid for the standardization of Gochang Bokbunja as a functional ingredient and health food were accomplished. A Symmetry$^{(R)}$ (C18, $4.6{\times}250mm$, $5.0{\mu}m$) column was used with a gradient elution system of 1% formic acid in water and acetonitrile. This method was validated according to specificity, linearity, accuracy, precision test, and recovery test. Specificity was confirmed with identical retention time, and calibration curves of ellagic acid showed good linear regression ($R^2$ >0.9996). Relative standard deviations (RSD) of data from the intra- and inter-day experiments were less than 2.28% and 2.84%, except in the low limit of quality control (LLOQ, $1{\mu}g/mL$) sample. The results of the recovery test were from 89.17% to 97.92% with RSD values from 0.05 to 0.14%. Therefore, we performed analysis of ellagic acid as a marker compound in Gochang Bokbunja extracts. The amount of ellagic acid in Gochang Bukbunja was about $1.918{\mu}g/mg$ (0.192%) in the three times analysis, and RSD was less than 2.36% by the validated method. These results suggest that the developed HPLC method is simple, efficient, and could contribute to the quality control of Gochang Bokbunja extract as a functional ingredient.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.1
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• pp.85-88
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• 2015

This study attempted to establish an HPLC analysis method for determination of marker compounds as a part of material standardization for the development of health functional food materials from Perilla frutescens Britton var. acuta Kudo. The quantitative determination method of rosmarinic acid as a marker compound of P. frutescens Britton var. acuta Kudo extract (PFE) was optimized by HPLC analysis using a C18 column ($4.6{\times}150mm$, $5{\mu}m$) with 0.1% acetic acid as the elution gradient and methanol as the mobile phase at a flow rate of 1 mL/min and detection wavelength of 280 nm. The HPLC/UV method was applied successfully to quantification of the marker compound in PFE 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 0.9995, and the limit of detection and limit of quantitation were $0.36{\mu}g/mL$ and $1.2{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 3.21% and 1.43%, respectively. Recovery rate test at rosmarinic acid concentrations of 12.5, 25 and $50{\mu}g/mL$ scored between 97.04~98.98% with RSD values from 0.25~1.97%. These results indicate that the established HPLC method is very useful for the determination of marker compound in PFE to develop a health functional material.

• Journal of Food Hygiene and Safety
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• v.39 no.2
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• pp.72-82
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• 2024

This study aimed to develop a scientifically and systematically standardized xylooligosaccharide analytical method that can be applied to products with various formulations. The analysis method was conducted using HPLC with Cadenza C₁₈ column, involving pre-column derivatization with 1-phenyl-3-methyl-5-pyrazoline (PMP) and UV detection at 254 nm. The xylooligosaccharide content was analyzed by converting xylooligosaccharide into xylose through acid hydrolysis. The pre-treated methods were compared and evaluated by varying sonication time, acid hydrolysis time, and concentration. Optimal equipment conditions were achieved with a mobile phase consisting of 20 mM potassium phosphate buffer (pH 6)-acetonitrile (78:22, v/v) through isocratic elution at a flow rate of 0.5 mL/min (254 nm). Furthermore, we validated the advanced standardized analysis method to support the suitability of the proposed analytical procedure such as specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision. The standardized analysis method is now in use for monitoring relevant health-functional food products available in the market. Our results have demonstrated that the standardized analysis method is expected to enhance the reliability of quality control for healthy functional foods containing xylooligosaccharide.