• Title/Summary/Keyword: RSD

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Method Validation and Quantification of Lutein and Zeaxanthin from Green Leafy Vegetables using the UPLC System (UPLC를 이용한 lutein과 zeaxanthin의 분석법 검증 및 엽채류에서의 정량적 평가)

  • Kim, Suna;Kim, Ji-Sun
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.686-691
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    • 2012
  • The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

Quantitative Analysis of Various Carotenoids from Different Colored Paprika Using UPLC (UPLC를 이용한 색상별 파프리카 유래 카로티노이드의 정량적 평가)

  • Hwang, Jeong Rok;Hwang, In Kyeong;Kim, Suna
    • Korean Journal of Food Science and Technology
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    • v.47 no.1
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    • pp.1-5
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    • 2015
  • This study aimed to simultaneously determine various carotenoids from different colored paprika using an ultra performance liquid chromatograph (UPLC) equipped with a HSS T3 column. Analysis was performed at 450 nm using gradient conditions with acetonitrile/methanol/methylene chloride (65/25/10) and distilled water. We improved the peak resolution and performed carotenoid analysis within 30 min. We qualitatively analyzed 11 carotenoids (neoxanthin, capsorubin, violaxanthin, capsanthin, zeaxanthin, lutein, ${\alpha}$-cryptoxanthin, ${\beta}$-cryptoxanthin, lycopene, ${\alpha}$-carotene, and ${\beta}$-carotene). For the validation of UPLC methods, we validated the precision and accuracy of capsanthin. Capsanthin showed good linearity ($R^2$=0.9998) in the concentration range of $1-200{\mu}g/mL$ with 2.4 and $7.2{\mu}g/mL$ of limit of detection (LOD) and limit of quantification (LOQ), respectively. The relative standard deviation (RSD) for intra- and inter-day precision was less than 3.83%. Recovery was in the range of 91.86-99.87%. We quantitatively analyzed carotenoid contents from 8 different colored paprika (red, orange, yellow, and green). The most abundant carotenoids were capsanthin in red paprika, and zeaxanthin in orange, yellow, and green paprika.

Validation of an analytical method of oxyresveratrol for standardization of Mulberry (Morus alba L.) branch extract as a functional ingredient (상지추출물의 기능성원료 표준화를 위한 지표성분 옥시레스베라트롤 분석법 검증)

  • Jeon, Young-Hee;Choi, Sang-Won
    • Korean Journal of Food Science and Technology
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    • v.50 no.4
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    • pp.377-382
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    • 2018
  • An HPLC method was developed to quantitate a marker, oxyresveratrol (ORT), for the standardization of mulberry branch extracts (MBE) as a functional ingredient. HPLC was performed on a $C_{18}$ column with a gradient elution using 0.05% $H_3PO_4$ and acetonitrile at a flow rate of 0.8 mL/min, and detected at 320 nm. The HPLC method was validated according to Korea Food and Drug Administration (KFDA) guideline of analytical procedures with respect to specificity, linearity, accuracy and precision. Calibration curve of ORT showed high linearity ($R^2=1$), and limits of detection and quantification were 0.3 and $1.0{\mu}g/mL$, respectively. Relative standard deviation values from intra-and inter-day precision were less than 3.52 and 4.70%, respectively. Recovery rate ranged from 97.64% to 103.69%, and ORT content in MBE was approximately 3.78%. These results suggest that the HPLC method developed for the analysis of ORT in MBE is simple, efficient, and could contribute to the quality control of MBE.

The preliminary evaluation of semi-quantitative analysis by in situ pre-chromatographic derivatization of amines and image analysis in TLC (TLC상 분리 전 직접적 유도체화 반응과 이미지 분석을 통한 아민 화합물의 반정량분석을 위한 선행평가)

  • Kim, Younsu;Choi, Sung-Woon
    • Analytical Science and Technology
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    • v.28 no.2
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    • pp.79-85
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    • 2015
  • A preliminary experiment was performed to develop a fast, convenient, and economical semi-quantitative method of analyzing amphetamine-like amines from images of derivatives. These were generated from the reaction (in situ, co-spot) of three amphetamine-like compounds with three derivatization reagents on a TLC plate. The attempt was made to optimize the reaction conditions for an efficient derivatization reaction, and TLC images taken by a digital camera were analyzed using two types of image analysis program (CP Atlas 2.0 and ImageJ) for repeatability (RSD, %) and linearity (R2). Then, their results were compared. For efficient derivatization, the reaction conditions needed to be modified. The results of image analysis of each of the samples at two different concentrations (0.5 mg/mL and 0.01 mg/mL) showed that the RSD values for reaction repeatability were in the range of 0.69-5.50%. From the calibration curves between the area of the derivative and the concentration of amines, the R2 values (R2 > 0.9906) for good linear correlation were found to be high, in a concentration range of 0.1-0.005 mg/mL of amines. In addition, the two programs demonstrated little difference in the analysis of repeatability and linearity of the derivatization, so that the current method has the potential to be used for the semi-quantitative analysis of amines.

Development of Enhanced Analytical Method for Perchlorate in Food by IC-MS/MS with an Internal Standard (IC-MS/MS와 내부표준물질을 이용한 식품 중 perchlorate 분석법 개선)

  • Yang, Min-June;Kim, Jong-Sung;Han, Jong-Hun;Her, Nam-Guk
    • Korean Journal of Food Science and Technology
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    • v.43 no.5
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    • pp.532-536
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    • 2011
  • The internal standard method using ion chromatography combined with tandem mass spectrometry (IC-MS/MS) for quantifying perchlorate in different types of food was established. Because the presence of ions and other biomolecules in matrices usually interrupts accurate determination of perchlorate, it is necessary to develop efficient, reproducible method to determine perchlorate concentrations in food. In this study, the internal standard method was compared with the external standard method to determine perchlorate concentrations in standard samples. The obtained method detection limit (MDL) for perchlorate was 0.005 ${\mu}g/L$ for bottled water, 0.12 ${\mu}g/L$ for milk, 0.27 ${\mu}g/kg$ for rice, 0.16 ${\mu}g/kg$ for vegetables, and 0.07 ${\mu}g/kg$ for seaweed, respectively. The limit of quantitation (LOQ) was calculated by multiplying the MDL by 7. The recoveries of perchlorate from food samples spiked with perchlorate ranged from 98 to 105% and their percent relative standard deviation (%RSD) levels were <20%. This method was successfully applied for the quantitative determination of perchlorate in various kinds of food.

Speciation Analysis of Arsenic Species in Surface Water (수중의 비소 종 분리 분석)

  • Jeong, Gwan-Jo;Kim, Dok-Chan
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.6
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    • pp.621-627
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    • 2008
  • In this study, a technique of speciation and determination of the trace inorganic arsenic(As(III) and As(V)) in water sample using HPLC-DRC-ICP-MS has been developed. Isocratic mobile phase of 10 mM ammonium nitrate and 10 mM ammonium phosphate monobasic was used and methanol(5 v/v%) was used as flushing solvent. Selection of the best flow rate of reaction gas, O$_2$, and optimization of the parameters such as pH and flow rate of mobile phase, and injection volume of sample for the separation and detection of arsenic species were carried out. The oxygen flow rate of 0.5 mL/min, pH of 9.4 and flow rate of 1.5 mL/min of mobile phase, and injection volume of sample of 100 $\mu$L were found to be the best parameters for the speciation and determination of arsenic species. The analytical features of the method were detection limit 0.10 and 0.08 $\mu$g/L, precision(RSD) 4.3% and 3.6%, and recovery 95.2% and 96.4% for As(III) and As(V), respectively. Analysis time was 4 minutes per sample. Linear calibration graphs with r$^2$ = 0.998 were obtained for both As(III) and As(V). Speciation analysis of arsenic species in the raw water samples collected from the tributary streams to Han River and main stream of Paldnag were performed by the proposed method. The concentrations of As(III) ranged from 0.10 to 0.22 $\mu$g/L and As(V) concentrations ranged from 0.44 to 1.19 $\mu$g/L, and 93.5% of total arsenic was found to be As(V).

Determination of Pyribencarb and Its Metabolite KIE-9749 in Agricultural Commodities by High-Performance Liquid Chromatography (액체크로마토그래피를 이용한 농산물중 pyribencarb와 대사물 KIE-9749의 잔류 분석법)

  • Kwon, Hyeyoung;Hong, Su-Myeong;Kim, Taek-Kyum;Kim, Hyung-Jin;Moon, Byeong-Chul;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.20 no.3
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    • pp.236-246
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    • 2016
  • The aim of this study was to develop an analytical method for the determination of pyribencarb and its metabolite KIE-9749 in agricultural commodities. The experiment was performed with a range of concentrations $0.05{\sim}2.5{\mu}g/g$ in apple, green pepper, potato, hulled rice, soybean, pear, peach, grape and cucumber. Each samples were extracted with acetone and cleaned by dichloromethane/saline water partition and purified with Florisil solid phase extraction (SPE) cartridge and aminopropyl SPE cartridge. Pyribencarb and KIE-9749 were separated and quantified by HPLC/UVD at 265nm using acetonitrile and water as mobile phase. The recoveries of pyribencarb and KIE-9749 were within 78.3~108.4% and 73.9~113.7% with RSD below 12.2% and 15.0%, respectively. The limits of quantification (LOQ) were both $0.05{\mu}g/g$. LC/ESI-MS/MS was optimized for confirmation of residue identity.

A Quantitative Method for Human Face Volume Using 3D Optical Measurement (3D 측정 기기를 이용한 얼굴의 부피 정량법 연구)

  • Park, Shin-Young;Nam,, Gae-Won;Kim, Seung-Hun;Lee, Hea-Kang;Ahn, Sung-Yeon;Moon, Seong-Joon;Kim, Han-Kon
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.4
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    • pp.333-338
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    • 2008
  • The evaluation for the visage volume was performed with human and dummy face using PRIMOS $body^{(R)}$. Three researchers measured the dummy face attached different volume of clay (6.6 mL, 13.2 mL, and 19.8 mL). It is identified that the high correlation between measured values and real volume ($R^2=0.99$). The percent (%) of relative standard deviation (RSD) of the data was shown below 10%. In Gage R&R analysis, the percent of contribution, the percent of study variation and distinct categories values were 0.78%, 8.85%, and 15% respectively. Therefore this method was regarded as the good standard condition in aspect of reproducibility and repetitiveness of data. The face volume variation was measured by PRIMOS $body^{(R)}$ on the face in participated 10 healthy Korean women volunteers. Subjects used the product once a day for two weeks as night sleeping pack. After application of the test products, the 3D image data of face were taken 1 and 2 weeks later. We found the face volume was significantly decreased after using products. In conclusion, this novel non-invasive technique was useful in measuring and visualizing alterations in face volume as a consequence of certain treatments. This system will provide a rapid and precise analysis of 3D topographical information for face.

A Study for Effects of Image Quality due to Scatter Ray produced by Increasing of Tube Voltage (관전압 증가에 기인한 산란선 발생의 화질 영향 연구)

  • Park, Ji-Koon;Jun, Je-Hoon;Yang, Sung-Woo;Kim, Kyo-Tae;Choi, Il-Hong;Kang, Sang-Sik
    • Journal of the Korean Society of Radiology
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    • v.11 no.7
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    • pp.663-669
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    • 2017
  • In diagnostic medical imaging, it is essential to reduce the scattered radiation for the high medical image quality and low patient dose. Therefore, in this study, the influence of the scattered radiation on medical images was analyzed as the tube voltage increases. For this purpose, ANSI chest phantom was used to measure the scattering ratio, and the scattering effect on the image quality was investigated by RMS evaluation, RSD and NPS analysis. It was found that the scattering ratio with increasing x-ray tube voltage gradually increased to 48.8% at 73 kV tube voltage and to 80.1% at 93 kV tube voltage. As a result of RMS analysis for evaluating the image quality, RMS value according to increase of tube voltage was increased, resulting in low image quality. Also, the NPS value at 2.5 lp/mm spatial frequency was increased by 20% when the tube voltage was increased by 93 kV compared to the tube voltage of 73 kV. From this study, it can be seen that the scattering radiation have a significant effect on the image quality according to the increase of x-ray tube voltage. The results of this study can be used as basic data for the improvement of medical imaging quality.

Determination of fucoxanthin in cosmeceutical products by HPLC-PDA (HPLC-PDA를 이용한 기능성 화장품 중 푸코잔틴의 정량)

  • Choi, Jongkeun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.12
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    • pp.755-761
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    • 2017
  • This study was conducted to establish an analytical method using an HPLC system equipped with a photodiode array (PDA) detector for the quality control of raw materials and cosmeceuticals containing fucoxanthin as an active ingredient. The column was octadecyl-functionalized silica gel and the measurement wavelength of the PDA was set to 499 nm. To validate the analytical method, the linearity of the calibration curve, detection limit, reproducibility and recovery rate were investigated and good results were obtained. The correlation coefficient of the calibration curve was 1.000 and the linearity was good in the concentration range of 0.5 ~ 100 ppm. Moreover, the limit of detection (LOD) was 0.1 ppm and the limit of quantification (LOQ) was 0.5 ppm. The results of the peak reproducibility test used for evaluating the system suitability showed that the RSD (n = 5) of the peak area was 2.0% and that of the retention time was 0.09%. In the spiking test, the recovery rate was $101.6{\pm}0.77%$. The fucoxanthin contents of the two kinds of fucoxanthin-containing raw materials were $49.6{\pm}3.3%$ and $1.03{\pm}0.016%$, respectively. In addition, the fucoxanthin content in the test product, which was intended to be 150 ppm, was $156.7{\pm}4.7ppm$. From the above results, it was concluded that this method could be applied to the quantitative analysis of fucoxanthin in cosmeceuticals.