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Development and Validation of an Analytical Method for Glucuronolactone in Energy Drinks by Hydrophilic Interaction Liquid Chromatography-electrospray Tandem Mass Spectrometry

  • Oh, Mi Hyune;Lim, Moo Song;Chai, Jeung Young;Kim, Eun Jung;Cho, Joong Hoon;Lim, Chul Joo;Choi, Sun Ok
    • 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.

Analytical Methods for Diethylstibestrol and Zeranol in Muscle Foods (근육 식품 중의 diethylstibestrol과 zeranol 분석법)

  • Ha, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.34 no.3
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    • pp.385-389
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    • 2002
  • Analytical method for diethylstibestrol (DES) and zeranol, which are growth promoters, in muscle foods was studied. Through selected ion monitoring analysis by GC-MSD for hormones, $M^+$ 412, 420, 416, and 433 for DES, $D_8DES$, ${\beta}-estradiol$, and zeranol, respectively, were selected for quantitative analysis. Removal of interferences in meat was done by passing the meat through 1 cc of strong anion exchanges resin, Dowex $2{\times}8$, 400 mesh, whereby the recoveries of DES and zeranol were achieved. Recoveries of DES and zeranol were ranged from 85 to 110%, and 75 to 110%, respectively, in meat using $D_8DES$ as an internal standard, while were 82 to 105%, and 65 to 120%, respectively, using ${\beta}-estradiol$ as an internal standard. These results show that both $D_8DES$ and ${\beta}-estradiol$ can be adopted as the internal standard for the analysis of DES and zeranol in muscle foods. Limits of detection of DES and zeranol were 0.05 and 1.0 ng/g, and limits of quantitation were 0.5 and 1.0 ng/g, respectively. The results of this study revealed no DES and zeranol were present in 14 samples of beefs, porks, ducks, chickens, mutiplicated flat fish, and trout.

Efficient 3D Object Simplification Algorithm Using 2D Planar Sampling and Wavelet Transform (2D 평면 표본화와 웨이브릿 변환을 이용한 효율적인 3차원 객체 간소화 알고리즘)

  • 장명호;이행석;한규필;박양우
    • Journal of KIISE:Computer Systems and Theory
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    • v.31 no.5_6
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    • pp.297-304
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    • 2004
  • In this paper, a mesh simplification algorithm based on wavelet transform and 2D planar sampling is proposed for efficient handling of 3D objects in computer applications. Since 3D vertices are directly transformed with wavelets in conventional mesh compression and simplification algorithms, it is difficult to solve tiling optimization problems which reconnect vertices into faces in the synthesis stage highly demanding vertex connectivities. However, a 3D mesh is sampled onto 2D planes and 2D polygons on the planes are independently simplified in the proposed algorithm. Accordingly, the transform of 2D polygons is very tractable and their connection information Is replaced with a sequence of vertices. The vertex sequence of the 2D polygons on each plane is analyzed with wavelets and the transformed data are simplified by removing small wavelet coefficients which are not dominant in the subjective quality of its shape. Therefore, the proposed algorithm is able to change the mesh level-of-detail simply by controlling the distance of 2D sampling planes and the selective removal of wavelet coefficients. Experimental results show that the proposed algorithm is a simple and efficient simplification technique with less external distortion.

Development of Simultaneous Analysis of Ferulic Acid, Caffeic Acid, Catechin and Taxifolin from Health Functional Food Pinus Pinaster Bark Extract by UPLC-MS/MS (건강기능식품 프랑스해안송껍질추출물 중 UPLC-MS/MS를 이용한 Ferulic acid, Caffeic acid, Catechin, Taxifolin 동시분석법 개발 연구)

  • Oh, Jae-Myoung;Kim, Ji An;Hu, Soo Jung;Choi, Yoon Hee;Oh, Keum Soon
    • 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).

Determining the residual surfactants in the fruits and vegetable washed with detergent (세척제를 사용한 과일 및 채소의 세척단계별 계면활성제 잔류량)

  • Lee, So Jeong;Park, Na-Youn;Kho, Young Lim;Kim, Jung Hoan
    • Korean Journal of Food Science and Technology
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    • v.53 no.6
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    • pp.792-798
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    • 2021
  • This study was conducted to determine the washing conditions in which surfactants were not detected after washing fruits and vegetables with detergent. Residual surfactants were analyzed using LC-MS/MS. The analyzed surfactants were LAS, SLES, AOS, SLS, CAPB, and LDAO. The survey found that 14% of the respondents used detergent correctly according to the directions indicated. After soaking the samples with 0.2% detergent, the average residual surfactant content was 2.61%. Soaking under 1% and 5% of the detergent, 4.68-5.50% of surfactant remained in the sample. In cherry tomatoes, the surfactants were below the LOD after rinsing twice. However, lettuce was rinsed three times. These results suggest that when using detergent for washing fruits and vegetables, following the labelled usage and rinsing at least three times in 30 seconds could minimize residual surfactants.

Locating QTLs controlling overwintering seedling rate in perennial glutinous rice 89-1 (Oryza sativa L.)

  • Deng, Xiaoshu;Gan, Lu;Liu, Yan;Luo, Ancai;Jin, Liang;Chen, Jiao;Tang, Ruyu;Lei, Lixia;Tang, Jianghong;Zhang, Jiani;Zhao, Zhengwu
    • Genes and Genomics
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    • v.40 no.12
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    • pp.1351-1361
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    • 2018
  • A new cold tolerant germplasm resource named glutinous rice 89-1 (Gr89-1, Oryza sativa L.) can overwinter using axillary buds, with these buds being ratooned the following year. The overwintering seedling rate (OSR) is an important factor for evaluating cold tolerance. Many quantitative trait loci (QTLs) controlling cold tolerance at different growth stages in rice have been identified, with some of these QTLs being successfully cloned. However, no QTLs conferring to the OSR trait have been located in the perennial O. sativa L. To identify QTLs associated with OSR and to evaluate cold tolerance. 286 $F_{12}$ recombinant inbred lines (RILs) derived from a cross between the cold tolerant variety Gr89-1 and cold sensitive variety Shuhui527 (SH527) were used. A total of 198 polymorphic simple sequence repeat (SSR) markers that were distributed uniformly on 12 chromosomes were used to construct the linkage map. The gene ontology (GO) annotation of the major QTL was performed through the rice genome annotation project system. Three main-effect QTLs (qOSR2, qOSR3, and qOSR8) were detected and mapped on chromosomes 2, 3, and 8, respectively. These QTLs were located in the interval of RM14208 (35,160,202 base pairs (bp))-RM208 (35,520,147 bp), RM218 (8,375,236 bp)-RM232 (9,755,778 bp), and RM5891 (24,626,930 bp)-RM23608 (25,355,519 bp), and explained 19.6%, 9.3%, and 11.8% of the phenotypic variations, respectively. The qOSR2 QTL displayed the largest effect, with a logarithm of odds score (LOD) of 5.5. A total of 47 candidate genes on the qOSR2 locus were associated with 219 GO terms. Among these candidate genes, 11 were related to cell membrane, 7 were associated with cold stress, and 3 were involved in response to stress and biotic stimulus. OsPIP1;3 was the only one candidate gene related to stress, biotic stimulus, cold stress, and encoding a cell membrane protein. After QTL mapping, a total of three main-effect QTLs-qOSR2, qOSR3, and qOSR8-were detected on chromosomes 2, 3, and 8, respectively. Among these, qOSR2 explained the highest phenotypic variance. All the QTLs elite traits come from the cold resistance parent Gr89-1. OsPIP1;3 might be a candidate gene of qOSR2.

Identification of Quantitative Trait Loci Associated with Resistance to Bacterial Pustule (Xanthomonas axonopodis pv. glycines) in Soybean (SSR 분자표지이용 콩 불마름병 저항성 관여 양적형질 유전자좌(QTL) 분석)

  • Seo, MinJung;Kang, Sung-Taeg;Moon, Jung-Kyung;Lee, Seukki;Kim, Yul-Ho;Jeong, Kwang-Ho;Yun, Hong-Tae
    • Korean Journal of Breeding Science
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    • v.41 no.4
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    • pp.456-462
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    • 2009
  • Bacterial pustule (BP), caused by Xanthomonas axonopodis pv. glycines, is prevalent disease in major soybean production areas. BP can reduce seed yield as well as seed quality. To identify the genomic region associated with the resistance to BP, QTL analysis was conducted using $F_{10}$ RIL (recombinant inbred lines) population, Keunolkong${\times}$Shinpaldalkong. Four QTLs for BP disease were identified on the linkage group B2, D2, I and K in field accounts for 36.4% of the phenotypic variation. Especially, QTL at near of Satt135 on LG D2 was identified in green house experiment explaining 20.9% of the phenotypic variation was found to be a major QTL conferring BP. One of these QTLs, Satt135 on the LG D2, was also identified in green house experiment. In both field and green house condition, the position of major QTL for BP was detected between Satt135 and Satt397 on the LG D2. The major QTL for BP may be used for minimizing soybean BP through effective marker-assisted selection (MAS).

Development and Validation of Analytical Method for Decursin in Aerial Parts of Angelica gigas Nakai Extract (참당귀 지상부 추출물의 지표성분 decursin의 분석법 개발 및 검증)

  • Kim, Hee-Yeon;Lee, Ki-Yeon;Kim, Tae-Hee;Park, A-Reum;Noh, Hee-Sun;Kim, Si-Chang;Ahn, Mun-Seob
    • 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.

Simultaneous Analysis of the Compounds of Natural Cosmetic Resources Containing Chrysanthemum zawadskii, Perilla frutescens, Rosa multiflora and their Anti-oxidative Activity (산구절초, 자소엽, 찔레를 함유한 천연 화장품소재의 다성분 동시분석과 항산화활성)

  • Ham, Ha Neul;Shrestha, Abinash Chandra;Kim, Ju Eun;Lee, Tae Bum;Yoo, Byoung Wan;Kim, Min Sook;Kim, Kwang Sang;Cha, Joon-Seok;Lee, Yong Mun;Kim, Jeong Yeob;Leem, Jae Yoon
    • Korean Journal of Pharmacognosy
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    • v.49 no.4
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    • pp.312-321
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    • 2018
  • Recently, consumer demand for functional cosmetics containing natural ingredients has been greatly expanded. To develop the natural cosmetic materials, we selected 3 plants, Chrysanthemum zawadskii Herbich (CZ), Perilla frutescens (L.) Britton var. acuta Kudo (PF), and Rosa multiflora Thunberg (RM) which showed high total flavonoid contents (TFC), total polyphenol contents (TPC), and strong DPPH radical scavenging effect. We determined astragalin, chlorogenic acid, and rosmarinic acid as a marker compound for quantitative analysis of the content of each material and standardization of the quality standards and manufacturing standards through LC/MS analysis. HPLC-DAD was used to simultaneously analyze these marker components of three natural product complexes (Mix) and to validate the analytical method through experiments such as linearity, accuracy and precision. The detection wavelengths were set at 210, 265, and 330 nm. The detected 3 compounds from extract of CZ, PF, RM showed significant linearity ($R^2${\geq_-}$0.9947). The limit of detection (LOD) of chlorogenic acid, astragalin and rosmarinic acid were $8.29{\mu}g/ml$, $2.28{\mu}g/ml$, and $27.00{\mu}g/ml$, respectively. The limit of quantification (LOQ) of chlorogenic acid, astragalin and rosmarinic acid were $25.11{\mu}g/ml$, $6.92{\mu}g/ml$, and $81.83{\mu}g/ml$, respectively. The contents of the three indicators of Mix were 19.82-24.71 mg/g of chlorogenic acid, 43.80-46.02 mg/g of astragalin, and 46.33-48.57 mg/g of rosmarinic acid.

A Study on the Migration of Heavy Metals from Polycarbonate Food Contact Materials Using an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) (식품용 폴리카보네이트 기구류 중 ICP-MS를 이용한 중금속 이행량 조사)

  • Park, Se-Jong;Park, So-Ra;Kim, MeeKyung;Choi, Jae Chun
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.24 no.3
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    • pp.107-112
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    • 2018
  • The purpose of this study was to investigate the migration levels of lead (Pb), cadmium (Cd) and arsenic (As) from polycarbonate food contact materials into food simulant at different temperatures ($70^{\circ}C$ and $100^{\circ}C$). The method was validated by linearity of calibration curves, limit of detection (LOD), limit of quantification (LOQ), recovery, precision and uncertainty. All of 200 samples, including bottles, cups, containers, ladles, spoons and tongs were purchased from domestic markets and analyzed by inductively coupled plasma mass spectrometry (ICP-MS). Mean concentrations of positive samples were higher at $100^{\circ}C$ than $70^{\circ}C$ as showing a dependency of migration temperature. The migration concentrations ranged from not-detected (ND) to $4.67{\mu}g/L$, ND to $0.49{\mu}g/L$L and ND to $2.91{\mu}g/L$ for Pb, Cd and As, respectively, which were far below the migration limits of Korea standards and specifications for food utensils, containers and packages.