• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.89-95
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• 2017

A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.431-437
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• 2019

This study was conducted to develop a simultaneous analysis method for ferulic acid, caffeic acid, catechin and taxifolin from Health Functional Food (HFF) Pinus Pinaster bark extract. The simultaneous analytical method for ferulic acid, caffeic acid, catechin and taxifolin is carried out using UPLC-MS/MS. The method validation was performed to determine selectivity, linearity, accuracy, limit of detection (LOD), limit of quantification (LOQ) and precision for ferulic acid, caffeic acid, catechin and taxifolin. LC-MS/MS method was established using an Acquity UPLC BEH $C_{18}$ Column and was applied for these 4 compounds. Product-ion traces, at m/z $194.2{\rightarrow}133$, $180.2{\rightarrow}135$, $290.3{\rightarrow}245$, $304.3{\rightarrow}248$, were used for quantitative analysis of ferulic acid, caffeic acid, catechin and taxifolin, respectively. Excellent linearity ($r^2=0.999$) was observed for ferulic acid, caffeic acid, catechin and taxifolin in the concentration range (50-2500 mg/L). The observed recoveries of these 4 compounds were found to be between 84.9 and 104.9%, while precision was between 1.20 and 4.43% relative standard deviation (% RSD).

• Korean Journal of Food Science and Technology
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• v.51 no.5
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• pp.420-424
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• 2019

An HPLC analysis method was developed and standardized for the detection of dieckol as a functional food ingredient in Ecklonia cava extracts. HPLC was performed using a Capcell Pak C18 column ($250{\times}4.6mm$, $5{\mu}m$) with a gradient elution of water and acetonitrile, both containing 0.1% (v/v) trifluoroacetic acid, at a flow rate of 1.0 mL/min at $25^{\circ}C$. The eluate was detected at 230 nm. For validation, the specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) of dieckol were measured. The calibration curve for the detection of dieckol had high linearity ($R^2=0.9994$), with LOD and LOQ values of 0.38 and $1.16{\mu}g/mL$, respectively. Recovery of the quantified compound ranged from 99.61 to 100.71%. The relative standard deviation values of the intra-day and inter-day precisions were less than 1.7 and 1.25%, respectively. These results indicate that the reported HPLC method is simple, reliable, and reproducible for the detection of dieckol in Ecklonia cava extracts.

• Journal of the Korean Society of Radiology
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• v.15 no.6
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• pp.789-794
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• 2021

Brachytherapy is a treatment in which radioactive isotopes are placed inside the body to intensively irradiate the tumor with radiation. Because brachytherapy uses a radioisotope source with a high dose rate, it is very important to know the exact location and dose of the source. However, in clinical practice, it is evaluated inaccurately with the naked eye through rulers and autoradiographs. Therefore, in this study, a dosimeter that can be used for brachytherapy was developed using a lead(II) iodide (PbI₂) material, and the applicability was evaluated by analyzing the reproducibility, linearity, and PID items. As a result of reproducibility evaluation, the RSD value was 1.41%, satisfying the evaluation criteria of 1.5%. As a result of the linearity evaluation, the R² value was 0.9993, which satisfies the evaluation criterion of 0.9990. As a result of PID evaluation, it showed only a difference of 0.06 cm compared with the theoretical value of the inverse square law of distance at the 50% dose reduction point. The dosimeter manufactured in this experiment shows results that satisfy the standard in all evaluations, so it is judged that the possibility of applying the dosimeter in the radiation brachytherapy area is sufficient.

• Journal of Food Hygiene and Safety
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• v.36 no.5
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• pp.376-381
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• 2021

Red beet (Beta vulgaris L.) is a root vegetable and a popular functional food ingredient of dark red-purple appearance due largely to betacyanins, principally betanine (75-95%) and its isomer, isobetanine (15-45%). This study developed an analytical method for beet red in terms of betanine and isobetanine in processed food products labeled with beet red as a food additive. High Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD) was used with a C₁₈ column. Linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision and uncertainty in measurement were calculated for method validation. Matrix-matched calibration was applied to the candy, ice cream, and cocoa product, respectively, and R² was ≥0.9998, showing a high level of linearity. The LOD and LOQ were 0.16 to 0.32 and 0.48 to 0.97 mg/L, respectively. As a result of repeated intra-day and interday experiments to validate the accuracy and precision of the analytical method, the recovery rates were 96.0-103.1% and 100.0-102.2%, respectively and the RSD% was 0.5-3.3% and 0.9-3.8%, respectively. Moreover, the measurement uncertainty was estimated to be 1.71-12.43% depending on the matrix and the measured concentration. In this study, betanine and isobetanine were quantified (8.4-3,823.4 mg/kg) by applying the developed analytical method to processed food products (n= 26; e.g., candy, ice cream, and other processed foods) labeled with beet red as a food additive.

• Journal of Food Hygiene and Safety
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• v.34 no.4
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• pp.334-339
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• 2019

A procedure based on high-performance liquid chromatography (HPLC) is described to determine ${\beta}-carotene$ in infant formulas. The method for ${\beta}-carotene$ analysis was performed on a C18 reversed-phase column using acetonitrile/methanol/dichloromethane (6:1:3, v/v/v) as a mobile phase. ${\beta}-Carotene$ was determined in HPLC with photo diode array (PDA) detector. The parameters of validation were specificity, linearity, LOD, LOQ, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity ($R^2$), which was over 0.999 in the range of 0.125~2 mg/L. The detection and quantification limits were 0.064 and 0.193 mg/L, respectively. The accuracy and precision of this method using an STD spiked sample were 80~119% and 1.02~2.05% respectively. The method was applied to the analysis of various infant formula and follow-up formulas products containing ${\beta}-carotene$, and all the products contained acceptable levels of ${\beta}-carotene$ for nutrition labeling.

• Korean Journal of Food Science and Technology
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• v.52 no.6
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• pp.580-586
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• 2020

Fishery resources have been widely consumed as protein- and vitamin-rich food sources in the Korean diet. However, information regarding their vitamin levels is extremely limited. In this study, trienzyme-Lactobacillus casei method was validated and used to determine the folate contents in fishery foods. The trienzyme-L. casei method for folate analysis showed excellent accuracy (85.2 to 95.3% recovery) and precision (repeatability 1.4% RSD and reproducibility 2.4% RSD). Folate contents of 20 fish foods (4 fish, 3 crustaceans, 3 sea algae, 3 cephalopods, 4 shellfish, and 3 others) ranged from 1.75 to 97.98 ㎍/100 g. Furthermore, we found that the folate content in seaweed fusiforme was the highest, followed by gulfweed (69.73 ㎍/100 g). Folate analysis using the trienzyme-L. casei method was determined excellent based on the z-score of -0.3 in the Food Analysis Performance Assessment Scheme test. Analytical and method validation data generated in this study could be used to update the national food composition table on vitamin B9 in Korean fishery resources.

• Journal of the Korean Society of Radiology
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• v.16 no.3
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• pp.211-216
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• 2022

In radiation therapy, accurate Quality Assurance (QA) is required to irradiate tumor tissue while minimizing damage to normal tissue. Therefore, a dosimeter that can accurately measure radiation is needed. The purpose of this study is to develop a highly efficient radiation dosimeter with high sensitivity by applying a particle in binder method that can reduce manufacturing costs and simplify processes to perovskite materials that are cheaper and simpler to manufacture. By evaluating the response characteristics to high-energy photon, the applicability of QA dosimeter to radiation therapy was evaluated. As a result of reproducibility evaluation, RSD at 6 MV energy was presented as 1.178% and 15 MV energy was presented as 1.141%. As a result of linearity evaluation according to linear regression analysis, R² values of 0.9999 were presented under each condition of 6 MV and 15 MV energy. It was found that the CsPbBr₃ dosimeter manufactured based on the results of reproducibility and linearity evaluation is highly applicable as a QA dosimeter in the field of therapeutic radiation. The CsPbBr₃ dosimeter manufactured in this study presented more than the standard performance in the evaluation of reproducibility and linearity, and it can be used as a radiotherapy QA dosimeter through improvement.

• Journal of Food Hygiene and Safety
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• v.37 no.5
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• pp.297-305
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• 2022

Antioxidants are food additives that extend the shelf life of food products by preventing lipid rancidity caused by active oxygen. They can either be naturally-derived or manufactured synthetically via chemical synthesis. In this study, method validation of five synthetic antioxidants, namely butylated hydroxyanisole, butylated hydroxytoluene, tertiary butylhydroquinone, propyl gallate, and disodium ethylenediaminetetraacetic acid, was performed using a high performance liquid chromatography-ultraviolet visible detector, and the method applicability was evaluated by analyzing foods containing antioxidants. The coefficient of determination (R²) average was 0.9997, while the limit of detection and limit of quantification were 0.02-0.53 and 0.07-1.61 mg/kg, respectively. The intra and inter-day accuracies and precisions were 83.2±0.7%-98.7±2.1% and 0.1%-5.7% RSD, respectively. Inter-laboratory validation for accuracy and precision was conducted using the Food Analysis Performance Assessment Scheme quality control material. The results satisfied the guidelines presented by the AOAC International. In addition, the expanded uncertainty was less than 16%, as recommended by CODEX. Consequently, to enhance public health safety, the results of this study can be used as basis data for evaluating the intake of synthetic antioxidants and assessing their risks in Korea.

• The Korea Journal of Herbology
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• v.28 no.6
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• pp.47-51
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• 2013

Objectives : The Illicii Veri Fructus was not only traditional medicine but also food in Asia. The aim of this study was selection of optimum solvent in the fruit of Illicii Veri Fructus because an appropriate solvent affect a medicinal effect. Methods : Illicii Veri Fructus was carried out ultrasonic-assisted extraction as various solvents. Two main compounds, p-anisaldehyde and anethole, were successfully analyzed by high performance liquid chromatography-photodiode array detector (HPLC-PDA) and carried out method validation according to ICH guideline. The optimum solvent selected by comparing with yields of two main ingredients. Results : The p-anisaldehyde and anethole were detected at approximately 8.0 min and 19.8 min, respectively. It was all below 5.0% that RSD of retention time and peak area for two main peaks. Calibration curves of two compounds were good linearity as $R^2$ >0.9999. All of the precisions and accuracy were good intra-day and inter-day as below 5.0% RSD. Limited of detection (LOD) of p-anisaldehyde and anethole were analyzed as $0.134{\mu}g/mL$ and $4.286{\mu}g$, respectively. Limited of quantification (LOQ) of two compounds were $0.407{\mu}g$ and $12.989{\mu}g$, respectively. As a result of this study, p-anisladehyde was detected as 0.209 ~ 0.467%, however anethole was not detected in the distilled water. Conclusions : Anethole was main component as 5.329 ~ 6.815% except for water extraction. Methanol extraction among various solvents was detected the highest contents of p-anisaldehyde and anethole as 0.467(${\pm}0.008$)% and 6.815(${\pm}0.220$)%, respectively.