• Title/Summary/Keyword: HPLC Chromatography

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Polyacetylene Compounds from Panax ginseng C.A. Meyer (인삼의 Polyacetylene 화합물)

  • Shim Sang Chul;Chang Suk-Ku
    • Proceedings of the Ginseng society Conference
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    • 1988.08a
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    • pp.122-128
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    • 1988
  • Several major polyacetylene compounds were isolated from the petroleum-ether fraction of fresh Korean ginseng roots through solvent fractionation. partition and silica gel column chromatography. Further separation of acetylenic compounds was accomplished by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The preparative separation for the various spectral measurements was carried out by low pressure preparative liquid chromatography. The chemical structure of these polyacetylenes separated was determined by UV. IR/FTIR. $^{1}H$ NMR. mass spectral and elemental analysis. These are identified to be heptadeca-1-en-4.6-diyn-3.9.l0.-triol [1] heptadeca-1.9-dien-4.6-diyn-3-ol. heptadeca-1.8-dien-4.6-diyn-3.10-diol and the 4th was denatured polyacetylene. heptadeca-1.4-dien-6.8-diyn-3.10-diol. Two different p-substituted benzoates of panaxynol were synthesized for the determination of exciton chirality. The circular dichroism spectra in the UV region show that panaxynol p-bromobenzoate and p-dimethyl-aminobenzoate constitute negative exciton chirality [2]. Isolated major polyacetylene compounds were irradiated in aerated solution with 300 nm UV light to obtain the oxidized product at the allylic alcohol center to corresponding carbonyl compounds such as heptadeca-1-en-4.6-diyn-9.10-diol-3-one and heptadeca-1.9-dien-4.6-diyn-3-one. These photooxidation compounds have en-on-diyne chromophore and undergo nucleophilic addition reaction with methanol to yield ${\beta}-methoxy$ carbonyl compounds such as heptadeca-9-en-4.6-diyn-1-methoxy-3-one and heptadeca-4.6-diyn-1-methoxy-9.10-diol-3-one.

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Reduction of Aflatoxin during the Cooking and Processing of Rice (쌀의 조리 및 가공 과정 중 Aflatoxin 감소에 관한 연구)

  • 여현종;김종규
    • Journal of Food Hygiene and Safety
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    • v.17 no.2
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    • pp.79-86
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    • 2002
  • Aflatoxin is a secondary fungal metabolite and is a public health hazard because it is a human carcinogenic and has many deleterious effects in men and animals. Rice is one of the better substrates far the fungus which can produce aflatoxins. This study was performed to investigate aflatoxin reduction during the cooking and processing of rice. Aflatoxin was produced by Aspergillus parasiticus ATCC 15517 on well-milled rice (Japonica type) at the level of 13.2 ppb. Cooked rice, rice cakes (baek-sol-gi, plain steamed rice bread), fermented rice (sikhye, sweet rice beverage), and popped rice were prepared from the aflatoxin-contaminated rice. Aflatoxin content in the samples was determined by high performance liquid chromatography. The total aflatoxin level was decreased to 46.9% in the cooked rice, 85.6% in the rice cakes, 11.4% in the fermented rice, and 7.6% in the popped rice, respectively (p.0.05). This reduction brought the level of aflatoxins down to below the Standard and Specification of korea (10 ppb), except for the rice cakes. These results indicate that washing, steaming, fermentation, and popping of rice was helpful in reducing the aflatoxin level in the rice and the most helpful factors were high temperature & high pressure. More research is needed to understand why the preparation of rice cakes did not reduce the level of aflatoxin as much as the other cooking methods.

Cardioprotective effect of ginsenoside Rb1 via regulating metabolomics profiling and AMP-activated protein kinase-dependent mitophagy

  • Hu, Jingui;Zhang, Ling;Fu, Fei;Lai, Qiong;Zhang, Lu;Liu, Tao;Yu, Boyang;Kou, Junping;Li, Fang
    • Journal of Ginseng Research
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    • v.46 no.2
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    • pp.255-265
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    • 2022
  • Background: Ginsenoside Rb1, a bioactive component isolated from the Panax ginseng, acts as a remedy to prevent myocardial injury. However, it is obscure whether the cardioprotective functions of Rb1 are related to the regulation of endogenous metabolites, and its potential molecular mechanism still needs further clarification, especially from a comprehensive metabolomics profiling perspective. Methods: The mice model of acute myocardial ischemia (AMI) and oxygen glucose deprivation (OGD)-induced cardiomyocytes injury were applied to explore the protective effect and mechanism of Rb1. Meanwhile, the comprehensive metabolomics profiling was conducted by high-performance liquid chromatography and quadrupole time-of-flight mass spectrometry (HPLC-Q/TOF-MS) and a tandem liquid chromatography and mass spectrometry (LC-MS). Results: Rb1 treatment profoundly reduced the infarct size and attenuated myocardial injury. The metabolic network map of 65 differential endogenous metabolites was constructed and provided a new inspiration for the treatment of AMI by Rb1, which was mainly associated with mitophagy. In vivo and in vitro experiments, Rb1 was found to improve mitochondrial morphology, mitochondrial function and promote mitophagy. Interestingly, the mitophagy inhibitor partly attenuated the cardioprotective effect of Rb1. Additionally, Rb1 markedly facilitated the phosphorylation of AMP-activated protein kinase α (AMPKα), and AMPK inhibition partially weakened the role of Rb1 in promoting mitophagy. Conclusions: Ginsenoside Rb1 protects acute myocardial ischemia injury through promoting mitophagy via AMPKα phosphorylation, which might lay the foundation for the further application of Rb1 in cardiovascular diseases.

Analysis of Components to Determine Illegal Premium Gasoline (가짜 고급휘발유 판정을 위한 성분 분석)

  • Lim, Young-Kwan;Kang, Byung-Seok;Lee, Bo-O-Mi;Park, So-Hwi;Park, Jang-Min;Go, Young-Hoon;Kim, Seung-Tae;Kang, Dea-Hyuk
    • Tribology and Lubricants
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    • v.37 no.6
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    • pp.232-239
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    • 2021
  • Petroleum is the most consumed energy source in Korea with a usage rate of 38.7% among the available primary energy sources. The price of liquid petroleum products in Korea includes taxes such as transportation·environment·energy tax. Thus, illegal production and distribution of liquid petroleum is widespread because of its huge price difference from that of the normal product and its tax-free nature. Generally, the illegal petroleum product is produced by mixing liquid petroleum with other similar petroleum alternatives. The two kinds of gasoline, common gasoline and premium gasoline, are being distributed in Korea. The premium gasoline is often adulterated with cheaper common gasoline that lowers the octane number of gasoline. It is possible to distinguish them with their color difference, green and yellow for different grade gasoline. However, when small volume of common gasoline is added to premium gasoline, it is difficult to determine whether premium gasoline contained common grade or not. In this study, we inspect gasoline, which is illegally produced by mixing common gasoline to premium gasoline. When the ratio of mixing common gasoline is increased, premium gasoline shows decreasing absorbance at 600 nm and 650 nm under UV-Vis spectrometer. Moreover, the detected intensity (mV·s) of green dye in high performance liquid chromatography (HPLC) was decreased by common gasoline under 0.99 correlation value. The more the common gasoline is mixed, the more olefin and naphthene are detected by gas chromatography. In addition, trimethyl pentane as octane improver, paraffin and toluene are decreased by common gasoline mixing. The findings of this study suggests that illegal petroleum can be identified by analysis of components and simulated samples.

Determination and Validation of Synthetic Antioxidants in Processed Foods Distributed in Korea

  • Park, Hyeon-Ju;Seo, Eunbin;Park, Jin-Wook;Yun, Choong-In;Kim, Young-Jun
    • 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.

BEEF MEAT TRACEABILITY. CAN NIRS COULD HELP\ulcorner

  • Cozzolino, D.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1246-1246
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    • 2001
  • The quality of meat is highly variable in many properties. This variability originates from both animal production and meat processing. At the pre-slaughter stage, animal factors such as breed, sex, age contribute to this variability. Environmental factors include feeding, rearing, transport and conditions just before slaughter (Hildrum et al., 1995). Meat can be presented in a variety of forms, each offering different opportunities for adulteration and contamination. This has imposed great pressure on the food manufacturing industry to guarantee the safety of meat. Tissue and muscle speciation of flesh foods, as well as speciation of animal derived by-products fed to all classes of domestic animals, are now perhaps the most important uncertainty which the food industry must resolve to allay consumer concern. Recently, there is a demand for rapid and low cost methods of direct quality measurements in both food and food ingredients (including high performance liquid chromatography (HPLC), thin layer chromatography (TLC), enzymatic and inmunological tests (e.g. ELISA test) and physical tests) to establish their authenticity and hence guarantee the quality of products manufactured for consumers (Holland et al., 1998). The use of Near Infrared Reflectance Spectroscopy (NIRS) for the rapid, precise and non-destructive analysis of a wide range of organic materials has been comprehensively documented (Osborne et at., 1993). Most of the established methods have involved the development of NIRS calibrations for the quantitative prediction of composition in meat (Ben-Gera and Norris, 1968; Lanza, 1983; Clark and Short, 1994). This was a rational strategy to pursue during the initial stages of its application, given the type of equipment available, the state of development of the emerging discipline of chemometrics and the overwhelming commercial interest in solving such problems (Downey, 1994). One of the advantages of NIRS technology is not only to assess chemical structures through the analysis of the molecular bonds in the near infrared spectrum, but also to build an optical model characteristic of the sample which behaves like the “finger print” of the sample. This opens the possibility of using spectra to determine complex attributes of organic structures, which are related to molecular chromophores, organoleptic scores and sensory characteristics (Hildrum et al., 1994, 1995; Park et al., 1998). In addition, the application of statistical packages like principal component or discriminant analysis provides the possibility to understand the optical properties of the sample and make a classification without the chemical information. The objectives of this present work were: (1) to examine two methods of sample presentation to the instrument (intact and minced) and (2) to explore the use of principal component analysis (PCA) and Soft Independent Modelling of class Analogy (SIMCA) to classify muscles by quality attributes. Seventy-eight (n: 78) beef muscles (m. longissimus dorsi) from Hereford breed of cattle were used. The samples were scanned in a NIRS monochromator instrument (NIR Systems 6500, Silver Spring, MD, USA) in reflectance mode (log 1/R). Both intact and minced presentation to the instrument were explored. Qualitative analysis of optical information through PCA and SIMCA analysis showed differences in muscles resulting from two different feeding systems.

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Analysis of coenzyme Q10 in human plasma by high performance liquid chromatography (고성능액체크로마토그라피를 이용한 혈장 내 코엔자임 큐텐 분석)

  • Park, Yong-Sun;Park, Sang-Boem;Song, Sean-Mi;Kim, Yong-Woo;Lee, Kyoung-Ryul
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.514-518
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    • 2009
  • Coenzyme $Q_{10}$($CoQ_{10}$), a vitamin E-like substance, represents a components of the complex antioxidant system of the human organism. $CoQ_{10}$ levels in human plasma were determined by high performance liquid chromatography (HPLC) with UV detection. It was dissociated from lipoproteins by methanol and extracted into n-hexane with liquid-liquid extraction procedure, after centrifugation, the supernatant was dried under nitrogen gas stream. The residue was dissolved in the absolute ethanol. Determination of $CoQ_{10}$ was performed on a $C_{18}$ reversed-phase analytical column with ultraviolet detection at 275 nm and the mobile phase containing 15% (v/v) ethanol in methanol at a flow rate of 1.7 mL/min. The low limit of quantitation was 0.02 mg/L (S/N=10), the linearity between the concentration and peak height is from 0.1 to 2.0 mg/L. Twenty-four randomly selected plasma samples from apparently healthy, 27 to 44 year old individuals (males and females) were analyzed for total $CoQ_{10}$. The average level in these subjects was $0.62{\pm}0.13mg/L$ with the range of 0.41-0.98 mg/L. This method has a specific and a sufficient limit of quantitation (LOQ) for analysis of $CoQ_{10}$ in human plasma in both a clinical study and research at laboratories.

Sensitive determination of paroxetine in canine plasma by liquid chromatography-tandem mass spectrometry (LC-MS/MS) (LC-MS/MS를 이용한 비글견 혈장 중 파록세틴의 고감도 분석)

  • Chang, Kyu Young;Kang, Seung Woo;Han, Sang Beom;Youm, Jeong-Rok;Lee, Kyung Ryul;Lee, Hee Joo
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.138-146
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    • 2007
  • A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.

Chemical profile and antioxidant activity of peel of Yellowball, a novel citrus variety

  • Sun Lee;Seong-Ho Jo;Ji-Hyun An;Seong-man Jeong;Dong-Shin Kim;Sang Suk Kim;Suk Man Park;Su Hyun Yun;Seung-Gab Han;Hyun-Jin Kim
    • Food Science and Preservation
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    • v.30 no.2
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    • pp.235-246
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    • 2023
  • Yellowball (Citrus hybrid cv. Yellowball ) is a new citrus hybrid between Haruka (C. tamurana × natsudaidai ) and Kiyomi (C. unshiu × sinensis) and is known to possess strong antioxidant activity. However, detailed information on the antioxidant components of its peel has not yet been reported. This study evaluated the antioxidant activity of the peel and identified the antioxidant components by fractionating a methanolic extract of Yellowball peels using liquid-liquid extraction with n-hexane, ethyl ether (ether), ethyl acetate (EA), butanol, and water. The phenolic contents and antioxidant activities of the n-hexane, ether, and EA fractions were higher than those of the other fractions, and these fractions were further separated by semi-preparative high-performance liquid chromatography (HPLC). Four antioxidant peaks, EA1, EA2, EA3, and He1, were isolated and analyzed using ultra-performance liquid chromatography-quadrupole-time- of-flight mass spectrometry (UPLC-Q-TOF MS). Sinapoyl glucoside and hesperidin were identified in EA2 and EA3, respectively, and a polymethoxylated flavone (PMF) complex (5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone, natsudaidain, tetrameth- oxyflavone, and tangeretin) was identified in He1. A compound in EA1 with m/z 223.0246 [M-H] could not be identified and was named unknown2. The antioxidant activity of unknown2 (IC50=69.17 ㎍/mL) was similar to that of Trolox, which was noted as a major antioxidant in Yellowball peel. Further studies on the antioxidant capacity of Yellowball peel are required; however, these results provide a foundation for using Yellowball peel as an antioxidant.

Flavonol glycosides from the flowers of Carthamus tinctorius and their anti-diabetic activity (잇꽃(Carthamus tinctorius)으로부터 Flavonol glycoside 화합물들의 분리 및 항당뇨 효과)

  • Bo-Ram Choi;Hyoung-Geun Kim;Yoon Hee Nam;Dahye Yoon;Woo Cheol Shin;Jin-Kyu Jang;Yunji Lee;Tong Ho Kang;Nam-In Baek;Dae Young Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.477-483
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    • 2023
  • The flowers of Carthamus tinctorius (Safflower) were extracted with 80% aqueous methanol (CTex) and the concentrates were partitioned into EtOAc (CTE), n-BuOH (CTB), and H2O (CTW) fractions. Repeated silica gel (SiO2) and octadecyl silica gel column chromatographies for the EtOAc and n-BuOH fractions led to isolation of four flavonol glycosides. Nuclear magnetic resornance, infrarad spectroscopy, and mass spectroscopy revealed the chemical structure of the isolated compounds, astragalin (1), isoquercetin (2), nicotiflorin (3), and rutin (4). Quantitative analysis of four isolated compounds in CTex was performed by HPLC. CTex was found to contain 1 at 0.107, 2 at 0.367, 3 at 6.752, and 4 at 0.991 mg/g, respectively. Through this study, an experiment was conducted to evaluate the protective effect on pancreatic islets of the extract, solvent fractions, and all isolated compounds using a zebrafish larvae damaged by alloxan. Pancreatic islet size treated with EtOAc (CTE), n-BuOH (CTB), and H2O (CTW) fractions and compounds 1-4 significantly increased compared to the alloxan-induced group. These results indicate that C. tinctorius flowers and its isolated compounds are used as potential anti-diabetic agents.