• Journal of the Society of Cosmetic Scientists of Korea
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• v.45 no.1
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• pp.69-75
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• 2019

Preservatives of cosmetics is managed by positive list in Korea. Positive list requires a proper quantitative analysis method, but the analysis method is still insufficient. In this study, gas chromatography with flame ionization detector was used to simultaneously analyze 14 preservatives in cosmetics. As a result of method validation, the specificity was confirmed by the calibration curves of 14 preservatives showing good linearity correlation coefficient of above 0.9997 except dehydroacetic acid (0.9891). The limits of detection (LOD) and quantification (LOQ) of 14 preservatives were 0.0001 mg/mL ~ 0.0039 mg/mL and 0.0003 mg/mL ~ 0.0118 mg/mL, respectively, but they were 0.0204 mg/mL, 0.0617 mg/mL for dehydroacetic acid, respectively. The precision (Repeatability) of the values was less than 1.0%, but 7.1% for dehydroacetic acid. The Accuracy (% recovery) of 14 preservatives in cosmetics showed 96.9% ~ 109.2%. Finally, this method was applied to 50 cosmetics available in market. Results showed that the commonly used preservatives were chlorophene, phenoxyethanol, benzyl alcohol and parabens. However, the amount of the detected preservatives was within maximum allowed limits established by KFDA.

• Korean Journal of Food Science and Technology
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• v.40 no.2
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• pp.152-159
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• 2008

The purpose of this study was to determine the accurate quantification of vitamin A in infant formula by comparing two different standard stock solutions as well as various sample weights using high performance liquid chromatography. The sources of uncertainty in measurement, such as sample weight, final smaple vloume, and the instrumental results, were identified and used as parameters to determine the combined standard uncertainty based on GUM(guide to the expression of uncertainty in measurement) and the Draft EURACHEM/CITAC Guide. The uncertainty components in measuring were identified as standard weight, purity, molecular weight, dilution of the standard solution, calibration curve, recovery, reproducibility, sample weight, and final sample volume. Each uncertainty component was evaluated for type A and type B and included to calculate the combined uncertainty. The analytical results and combined standard uncertainties of vitamin A according to the two different methods of stock solution preparation were 627 ${\pm}$ 33 ${\mu}$g R.E./100 g for 1,000 mg/L of stock solution, and 627 ${\pm}$ 49 ${\mu}$g R.E./100 g for 100 mg/L of stock solution. The analytical results and combined standard uncertainties of vitamin A according to the various sample weighs were 622 ${\pm}$ 48 ${\mu}$g R.E./100 g, 627 ${\pm}$ 33 ${\mu}$g R.E./100 g, and 491 ${\pm}$ 23 ${\mu}$g R.E./100 g for 1 g, 2 g, and 5 g of sampling, respectively. These data indicate that the preparation method of standard stock solution and the smaple amount were main sources of uncertainty in the analysis results for vitamin A. Preparing 1,000 mg/L of stock solution for standard material sampling rather than 100 mg, and sampling not more than 2 g of infant formula, would be effective for reducing differences in the results as well as uncertainty.

• Journal of The Korean Society of Grassland and Forage Science
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• v.36 no.4
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• pp.333-339
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• 2016

The objective of this study was to optimize analytical methods for ochratoxin A (OTA) and zearalenone (ZEA) in rice straw silage and winter forage crops using ultra-high performance liquid chromatography (UHPLC). Samples free of mycotoxins were spiked with $50{\mu}g/kg$, $250{\mu}g/kg$, or $500{\mu}g/kg$ of OTA and $300{\mu}g/kg$, $1500{\mu}g/kg$, or $3000{\mu}g/kg$ of ZEA. OTA and ZEA were extracted by acetonitrile and cleaned-up using an immunoaffinity column. They were then subjected to analysis with UHPLC equipped with a fluorescence detector. The correlation coefficients of calibration curves showed high linearity ($R^2{\geq_-}0.9999$ for OTA and $R^2{\geq_-}0.9995$ for ZEA). The limit of detection and quantification were $0.1{\mu}g/kg$ and $0.3{\mu}g/kg$, respectively, for OTA and $5{\mu}g/kg$ and $16.7{\mu}g/kg$, respectively, for ZEA. The recovery and relative standard deviation (RSD) of OTA were as follows: rice straw = 84.23~95.33%, 2.59~4.77%; Italian ryegrass = 79.02~95%, 0.86~5.83%; barley = 74.93~97%, 0.85~9.19%; rye = 77.99~96.67%, 0.33~6.26%. The recovery and RSD of ZEA were: rice straw = 109.6~114.22%, 0.67~7.15%; Italian ryegrass = 98.01~109.44%, 1.65~4.81%; barley = 98~113.53%, 0.25~5.85%; rye = 90.44~108.56%, 2.5~4.66%. They both satisfied the standards of European Commission criteria (EC 401-2006) for quantitative analysis. These results showed that the optimized methods could be used for mycotoxin analysis of forages.

• Korean Journal of Food Science and Technology
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• v.51 no.6
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• pp.517-523
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• 2019

In this study, we investigated antioxidant capacity of 20 strawberry extract using the DPPH and ABTS assay and HPLC-DAD validation method. The total polyphenolic and flavonoids contents of 20 strawberry extracts were 22.77-107.61 mg TAE/100 g FW and 17.58-44.12 mg QE/100 g FW. The Aiberry and Elie star showed the highest total polyphenol and flavonoid contents, respectively. The DPPH radical scavenging activity of what was 1540.6-1124.0 μmol TEAC/100 g FW and Derunoka showed the highest activity. The ABTS radical scavenging activity was 6352.3-4592.3 μmol TEAC/100 g FW and FA23 showed the highest activity. The HPLC-DAD method for the quantitation of ellagic acid results showed high linearity in various concentration ranges, and the limit of detection was 2.35 μg/mL. The limit of quantification was 7.12 μg/mL. Relative standard deviation values from intra-and inter-day precision were less than 5.31%. Recovery rate at 10, 50, and 100 μg/mL, respectively, were 100.0-101.0% with relative standard deviation (RSD) values less than 5.30%. These results provide viable information for the validation of antioxidant capacity in strawberry fruits.

• Journal of Food Hygiene and Safety
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• v.33 no.4
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• pp.289-295
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• 2018

The aim of this study was to develop and validate an analytical method for determining the presence of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for wogonin, quercetin, and quercetin-3-O-glucuronide using high performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for wogonin, quercetin, and quercetin-3-O-glucuronide were 0.9999. The LOD for wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.09 to 0.16 and those for the LOQ ranged from 0.26 to $0.48{\mu}g/mL$. The inter-day and intra-day precision values of wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.74 to 1.87 and from 0.28 to 1.12%, respectively. The inter-day and intra-day accuracies were 99.96~115.88% and 99.73~114.81%, respectively. Therefore, the analytical method was validated for the detection of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures.

• Analytical Science and Technology
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• v.31 no.4
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• pp.161-170
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• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.5
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• pp.680-689
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• 2016

The present study evaluated the validation method for isoflavone contents of fermented soybean extracts by bioconversion as well as their antioxidant activities. Our results show that the total isoflavone contents of non-fermented and fermented soybean extract ranged between 119.8 to $637.7{\mu}g/g$ and between 567.3 to $2,074.6{\mu}g/g$, respectively. Moreover, fermented soybean extracts had higher contents of isoflavone aglycones, including daidzein, glycitein, and genistein than non-fermented soybean extracts as well as lower contents of isoflavone glucosides such as daidzin, glycitin, and genistin. FRAP and ORAC values ranged between 0.15 to 0.22 and between 195.24 to $753.79{\mu}M$ Trolox equivalents/g in non-fermented and fermented soybean extracts, respectively. These results indicate that fermented soybean extracts had higher total isoflavone contents and antioxidant activities than non-fermented soybean extracts. Bioconversion process in this study may have the potential to produce isoflavone-enriched natural antioxidant agents with high added value from soybean matrices.

• Journal of Food Hygiene and Safety
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• v.20 no.3
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• pp.141-146
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• 2005

A simple and sensitive analysis method based on reverse phase (RP) HPLC with UV detector was developed for simultaneous determination of chlorophyll a and b, pheophorbide a and $\beta-Carotene$ in Chlorella and Spirulina products. For added concentration $(50\;\mug/ml)$ of chlorophyll a and b, pheophorbide a and $\beta-Carotene$, recoveries of those were 70.3, 71.6, 60.1 and $90.5\%$, respectively, with relative standard deviations of 2.8,6.0, 10.6 and $10.4\%$. Limit of detection and quantification had ranges of $0.1\sim1.0\;\mug/ml$ and $0.2\sim2.0\;\mug/ml$, respectively. Calibration curve was linear with correlation coefficient of 0.995 for chlorophyll a and b, pheophorbide a and $\beta-Carotene$. Results of simultaneous determination in Chlorella and Spirulina products were showed ranges of $121.g\sim543.0\;\mug/ml$ for chlorophyll a,$0.6\sim160.0\;\mug/ml$ for chlorophyll b, $19.2\sim60.3\;\mug/ml$ for pheophorbide a and $383.6\sim1713.7\;\mug/ml$ for $\beta-Carotene$, respectively. Chlorophyll b contents in Chlorella products were detected above 30 times level to those in Spirulina products. $\beta-Carotene$ contents in Spirulina products were detected 2.7 times level to those in Chlorella products.

• Journal of Food Hygiene and Safety
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• v.35 no.3
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• pp.225-233
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• 2020

By the standards and specifications for hygiene products, three test methods for formaldehyde are specified for each item type of hygiene product. After derivatization using acetylacetone and 2,4-dinitrophenylhydrazine (2,4-DNPH), formaldehyde is analyzed by spectrophotometer and high-performance liquid chromatography (HPLC). Validation of the three test methods was performed on tissue, diaper lining and waterproof layer, and panty liner products. The results of linearity (R²), limit of detection (LOD), limit of quantification (LOQ), recovery rate (%) and reproducibility (%), showed that all three methods are suitable for analyzing formaldehyde in hygiene products. After derivatization with 2,4-DNPH and cetylacetone, formaldehyde was analyzed at 0, 3, 6, 9, 24 and 48 hours by HPLC. Formaldehyde derivatized with 2,4-DNPH showed no statistically significant change in formaldehyde peak area over time (P>0.05). But, acetylacetone-derivatizated formaldehyde showed a negative correlation coefficient (r) over time (P<0.01). We investigated the residual amounts of formaldehyde in 205 hygiene products distributed in Busan. Among 74 disposable diaper products tested, 73 had low concentrations of formaldehyde (0.13-29.87 mg/kg). Moreover, formaldehyde was not detected in any of 78 tissue, 27 disposable paper towel, 12 disposable dishcloth, 7 paper cup, one brand of paper straw and 6 disposable napkin products.

• 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%.