• Title/Summary/Keyword: LC-MS/MS analysis

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Development of an Analytical Method for the Determination of Pyriofenone residue in Agricultural Products using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 살균제 pyriofenone 분석법 확립)

  • Park, Hyejin;Kim, HeeJung;Do, Jung-Ah;Kwon, Ji-Eun;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.18 no.2
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    • pp.79-87
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    • 2014
  • Pyriofenone is an aryl phenyl ketone fungicide that is newly registered in Korea in 2013 to control powdery mildew on food. The objective of this study was to develop reliable and sensitive analytical method for determination of pyriofenone residue in agricultural products for ensuring the food safety. The pyriofenone residues in all samples(Korean melon, pepper, potato, mandarin, soybean, and hulled rice) were extracted with acetonitrile, partitioned with dichloromethane, and then purified with a silica cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of pyriofenone was 0.05~5 mg/kg with the correlation coefficient ($r^2$) > 0.999. Average recoveries of pyriofenone ranged from 72.8% to 99.5% at the spiked level of 0.05 and 0.5 mg/kg, while the relative standard deviation was 2.3%~6.4%. In addition, the limit of detection and limit of quantification were 0.01 and 0.05 mg/kg, respectively. The results revealed that the developed and validated analytical method was suitable for pyriofenone determination in agricultural products.

Determination of Heterocyclic Amines in Roasted Fish and Shellfish by Liquid Chromatography-Electrospray Ionization/Mass Spectrometry (Liquid chromatography-mass spectrometry를 이용한 가열 조리된 어패류에서의 heterocyclic amines 함량 분석)

  • Lee, Jae-Hwan;Back, Yoo-Mi;Lee, Kwang-Geun;Shin, Han-Seung
    • Korean Journal of Food Science and Technology
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    • v.41 no.3
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    • pp.326-333
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    • 2009
  • Heterocyclic aromatic amines (HCAs) are mutagenic and carcinogenic substances that are formed during the heating of protein-rich foods. HCAs are generally found at low amounts in a complex matrix, which requires sophisticated analysis. In this study, HCAs were extracted from lyophilized fish and shellfish samples using solid-phase extraction (SPE) and determined by liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI-MS). The HCA recoveries in the fish and shellfish ranged from 15.7 to 74.7% with standard deviations from 0.2 to 7.63%. And HCA concentrations ranged from 0.8 to 1,117.7 $ng/g^{-1}$ in cooked food samples. 1-methyl-9H-pyrido[3,4-b]indole (Harman), 9H-pyrido[3,4-b]indole (Norharman), and 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) were the most abundant HCAs formed in the muscle of fried mackerel, at levels of 1,117.7, 926.6, and 133.7 ng/g, respectively. 3-amino-1-methyl-5H-pyrido[4,3-b]indole (Trp-P-2), 2-aminodipiryrido[1,2-a:3,2-d]imidazole(Glu-P-2), 2-amino-9H-pyrido[2,3-b]indole(A${\alpha}$C), 2-amino-3methyl-9H-pyrido [1,2-a:3,2-d]imidazole(MeA${\alpha}$C), 2-amino-3,4,7,8-tetramethylimidazo[4,5-f]quinoxaline (TriMeIQx), 2-amino-3,7,8-trimethylimidazo [4,5-f]quinoxaline(7,8-DiMeIQx), and 2-amino-3,8-dimethylimidazo[4,5-f]quinoxaline (MeIQx) were only detected by small quantities ranged from 1.5 to 98.6 ng/g. Overall, this study provides useful information on HCA levels in fish and shellfish products consumed in Korea.

Analysis of Medroxyprogesterone Acetate in Meats (유통 식육 중 성장호르몬제 초산메드록시프로게스테론의 분석)

  • Lee, Yoon-Ae;Shim, Jee-Youn;Lee, Ryun-Kyung;Kim, Seung-Hwan;Oh, Hyun-Sook;Cho, Tae-Yong
    • Journal of Food Hygiene and Safety
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    • v.25 no.3
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    • pp.226-231
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    • 2010
  • We aimed at the monitoring medroxyprogesterone acetate (MPA) residue amount in meats and confirmed the safety of its residue in meats. Optimized condition for analytical and instrumental methods was obtained by method validation. The limit of detection (LOD) and limit of quantification (LOQ) were validated at 1.5 and 5.0 ug/kg, respectively. The calibration curve showed good linearity ($r^2$ = 0.9968) within the concentration range of 5.0~50.0 ug/kg. We selected progesterone-d9 for internal standard, The recoveries in fortified meat ranged from 67.5 to 109.56% at the 3 spiking levels. As the regulation of MPA analysis method used by LC-MS/MS on other products have established. We selected 3 species of farm stock products (cattle, pig, chicken) and purchased at the markets of seven major cities. The total 196 of meat including 46 of domestic beef, 43 of import beef, 60 of domestic pork, 12 of import pork and 35 of domestic chicken. No residue of synthetic growth hormones were detected in cattle, pig and chicken samples tested.

A Study on the Safety of Mycotoxins in Grains and Commonly Consumed Foods (곡류 등 다소비 식품 중 곰팡이독소 안전성 조사 연구)

  • Kim, Jae-Kwan;Kim, Young-Sug;Lee, Chang-Hee;Seo, Mi Young;Jang, Mi Kyung;Ku, Eun-Jung;Park, Kwang-Hee;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.32 no.6
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    • pp.470-476
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    • 2017
  • The purpose of this study was to investigate and evaluate the safety of the grains, nut products, beans and oilseeds being sold in Gyeonggi province by analyzing mycotoxins. A multi-mycotoxins analysis method based on LC-MS/MS was validated and applied for the determination of eight mycotoxins, including aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$), fumonisins ($B_1$, $B_2$), zearalenone and ochratoxcin A in 134 samples. The limit of detection (LOD) and limit of quantitation (LOQ) for the eight mycotoxins ranged from 0.14 to $8.25{\mu}g/kg$ and from 1.08 to $7.21{\mu}g/kg$, respectively. Recovery rates of mycotoxins were determined in the range of 61.1 to 97.5% with RSD of 1.0~14.5% (n=3). Fumonisin $B_1$, $B_2$, zearalenone, and ochratoxin A were detected in 22 samples, indicating that 27% of grains, 12.5% of beans and 11.8% of oilseeds were contaminated. Fumonisin and zearalenone were detected simultaneously in 2 adlays and 3 sorghums. Fumonisin $B_1$ and $B_2$ were detected simultaneously in most samples whereas fumonisin $B_1$ was detected in 1 adlay, 1 millet and 1 sesame sample. The average detected amount of fumonisin was $49.3{\mu}g/kg$ and $10.1{\mu}g/kg$ for grains and oilseeds, respectively. The average detected amount of zearalenone was $1.9{\mu}g/kg$ and $1.5{\mu}g/kg$ for grains and beans, respectively. In addition, the average amount of ochratoxin A was $0.08{\mu}g/kg$ for grains. The calculated exposure amounts of fumonisin, zeralenone and ochratoxin A for grains, beans and oilseeds were below the PMTDI/PTWI.

Proteomic analysis for the effects of non-saponin fraction with rich polysaccharide from Korean Red Ginseng on Alzheimer's disease in a mouse model

  • Sujin Kim;Yunkwon Nam;Min-jeong Kim;Seung-hyun Kwon;Junhyeok Jeon;Soo Jung Shin;Soyoon Park;Sungjae Chang;Hyun Uk Kim;Yong Yook Lee;Hak Su Kim;Minho Moon
    • Journal of Ginseng Research
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    • v.47 no.2
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    • pp.302-310
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    • 2023
  • Background: The most common type of dementia, Alzheimer's disease (AD), is marked by the formation of extracellular amyloid beta (Aβ) plaques. The impairments of axons and synapses appear in the process of Aβ plaques formation, and this damage could cause neurodegeneration. We previously reported that non-saponin fraction with rich polysaccharide (NFP) from Korean Red Ginseng (KRG) showed neuroprotective effects in AD. However, precise molecular mechanism of the therapeutic effects of NFP from KRG in AD still remains elusive. Methods: To investigate the therapeutic mechanisms of NFP from KRG on AD, we conducted proteomic analysis for frontal cortex from vehicle-treated wild-type, vehicle-treated 5XFAD mice, and NFP-treated 5XFAD mice by using nano-LC-ESI-MS/MS. Metabolic network analysis was additionally performed as the effects of NFP appeared to be associated with metabolism according to the proteome analysis. Results: Starting from 5,470 proteins, 2,636 proteins were selected for hierarchical clustering analysis, and finally 111 proteins were further selected for protein-protein interaction network analysis. A series of these analyses revealed that proteins associated with synapse and mitochondria might be linked to the therapeutic mechanism of NFP. Subsequent metabolic network analysis via genome-scale metabolic models that represent the three mouse groups showed that there were significant changes in metabolic fluxes of mitochondrial carnitine shuttle pathway and mitochondrial beta-oxidation of polyunsaturated fatty acids. Conclusion: Our results suggested that the therapeutic effects of NFP on AD were associated with synaptic- and mitochondrial-related pathways, and they provided targets for further rigorous studies on precise understanding of the molecular mechanism of NFP.

Physicochemical Characteristics of Cultivated Aromatic Rice Germplasm and Comparative Analysis of Flavor Components During Transplanting Time (국내 육성된 향미 품종의이앙시기별 이화학적 특성 및 향기성분 비교 분석)

  • Cho, Jun Hyun;Song, You Chun;Lee, Kwang Sik;Choi, Sik Won;Lee, Mi Ja;Jang, Ki Chang;Kim, Hyun Young;Kang, Hyeon Jung;Park, Ki Do;Seo, Woo Duck
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.175-183
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    • 2017
  • BACKGROUND:The Aromatic rice which is characterized by the flavor of Nurungji when cooked rice, and consumption is increasing recently. The purpose of this study was to investigate the physicochemical characteristics and aroma components of five aromatic rice cultivars according to transplanting time. METHODS AND RESULTS: Quantitative analysis of protein, fat, fatty acid and essential amino acid for five aroma rice cultivars(Hyangmibyeo 2 ho, Aromi, Mihyang, Aranghyangchal, Heughyang)and transplanting time was analyzed by crude protein analyzer, gas chromatography (GC), liquid chromatography (LC) and viscosity analysis was done by using rapid viscosity analyzer (RVA). The content of 2-acetyl-1-pyrroline (2AP) was determined by gas chromatography mass spectrometer. (GC-MS) As a result, the average protein and lipid contents were 6.5% and 2.4%, respectively. The content of essential amino acid showed the highest content at 104.4mg/g. There was no significant change in normal nutrients during the transplanting time. By RVA, cv.Hyangmibyeo 2 ho showed the highest peak and total setback viscosities and lowest breakdown viscosity in early transplantation. The content of 2AP in flavor varieties and transplanting time was quantitatively analyzed by GC-MS. Among the cultivars, Aromi showed the highest 2AP contents at $66.7{\mu}g/100gin$ normal transplanting time. CONCLUSION: cv.Aromi and Hyangmibyeo 2 ho were excellent physicochemical properties and 2AP components contents amongaromatic rice cultivars tested. Theiroptimaltime to transplant was at the beginning of June in the area of Miryang.

Simultaneous Determination of Synthetic Phosphodiesterase-5 Inhibitors in Dietary Supplements by Liquid Chromatography-High Resolution/Mass Spectrometry

  • Kim, So-Hee;Kim, Ho-Jun;Son, Jung-Hyun;Jeon, Byoung-Wook;Jeong, Eun-Sook;Cha, Eun-Ju;Lee, Jae-Ick
    • Mass Spectrometry Letters
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    • v.3 no.2
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    • pp.50-53
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    • 2012
  • After success of sildenafil for the treatment of erectile dysfunction, a large number of its analogues have been approved from FDA. Recently, the illegal dietary supplements which include sildenafil, vardenafil, tadalafil, or analogues of these drugs as ingredient have been widely distributed. Therefore, the determination of the residue of synthetic phosphodiesterase- 5 (PDE-5) inhibitors in dietary supplements is highly required due to indiscriminate and unintentional overdose caused nausea, chest pains, fainting and irregular heartbeat. In this paper, we report a rapid and sensitive analytical method for the simultaneous determination of nine phosphodiesterase-5 inhibitors by liquid chromatography-high resolution mass spectrometry. The present method was found to be accurate and reproducible with 40 ${\mu}g$/g of the limit of quantification for the nine PDE-5 inhibitors. The developed method can be successfully applied to the analysis of the seven illegal dietary supplements.

Dyeing Properties of Microbial Violacein on Mutifiber Fabrics (미생물 violacein 색소의 다섬교직포에서의 염색성)

  • Choi, Jong-Myoung;Kim, Yong-Sook
    • Fashion & Textile Research Journal
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    • v.11 no.5
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    • pp.818-826
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    • 2009
  • Dyeability of microbial violacein produced from Chromobacterum violaceum CV107 on to multifiber fabrics has been studied. The bluish-purple colourants were produced by cultivation of Chromobacterum violaceum using LB liquid medium for 2 days. The colourant was extracted with 80% acetone and identified as violacein by LC/MS analysis. The violacein could be dyed on not only natural fibers such as Cotton, Silk and Wool but also synthetic fibers such as Diacetate, Triacetate, Creslan 61 and Nylon 66. Maximum K/S values were shown at 540-580 nm according to different fiber with color appearance of purple or blue. An optimum pH and temperature under dyeing condition were 10 and $70^{\circ}C$, respectively. Any mordants were not improved colour density and quality on various fabrics. From this studies, pigments produced microbe have a high potentials for natural dyeing on fabrics. Finally, development of new colourants from microbe has made a possible change for new dyeing field in respects of eco-friend and repeatability of natural dyeing for apparels.

Isolation of Hyaluronidase Inhibitory Component from the Roots of Astraglus membranaceus Bunge (Astragali Radix)

  • Lee, Yun-Mi;Choi, Soo-Im;Lee, Jae-Won;Jung, Sun-Mi;Park, Sang-Min;Heo, Tae-Ryeon
    • Food Science and Biotechnology
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    • v.14 no.2
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    • pp.263-267
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    • 2005
  • In order to isolate hyaluronidase (HAase) inhibitor from Astragali radix (AR), dried roots were extracted with ethanol, prior to sequential fractionations with n-hexane, chloroform, ethyl acetate, n-butanol, and aqueous fractions. The n-butanol soluble fraction was found to exhibit the most pronounced inhibitory effect (68%) on HAase, and the active components were separated using various chromatographic methods, including column chromatography and preparative HPLC. The active component was isolated from the n-butanol soluble fraction of AR and was structurally identified as calycosin-7-O-${\beta}$-D-glucopyranoside by LC-MS, IR, $^1H$ NMR, and $^{13}C$ NMR analysis. The $IC_{50}$ of calycosin-7-O-${\beta}$-D-glucopyranoside's HAase activity was found to be 3.7 mg/mL.

Comparison of linear and non-linear equation for the calibration of roxithromycin analysis using liquid chromatography/mass spectrometry

  • Lim, Jong-Hwan;Yun, Hyo-In
    • Korean Journal of Veterinary Research
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    • v.50 no.1
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    • pp.11-17
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    • 2010
  • Linear and non-linear regressions were used to derive the calibration function for the measurement of roxithromycin plasma concentration. Their results were compared with weighted least squares regression by usual weight factors. In this paper the performance of a non-linear calibration equation with the capacity to account empirically for the curvature, y = ax$^{b}$ + c (b $\neq$ 1) is compared with the commonly used linear equation, y = ax + b, as well as the quadratic equation, y = ax$^{2}$+ bx + c. In the calibration curve (range of 0.01 to 10 ${\mu}g/mL$) of roxithromycin, both heteroscedasticity and nonlinearity were present therefore linear least squares regression methods could result in large errors in the determination of roxithromycin concentration. By the non-linear and weighted least squares regression, the accuracy of the analytical method was improved at the lower end of the calibration curve. This study suggests that the non-linear calibration equation should be considered when a curve is required to be fitted to low dose calibration data which exhibit slight curvature.