• Title/Summary/Keyword: high performance liquid chromatography

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Development of Analytical Method for Rutin in Buckwheat Plant using High Performance Liquid Chromatography (메밀 식물체 함유 Rutin의 HPLC 분석방법 개발)

  • Choung Myoung-Gun
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.50 no.spc1
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    • pp.181-186
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    • 2005
  • This experiment was conducted to know the appropriate methods for extraction and determination of rutin contained buckwheat plants. The efficient HPLC analytical condition of rutin contained buckwheat plants was developed. The gradient elution employed a $250mm\times4.6mm$ i.d. Tosoh ODS 120T column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of $2\%$ Acetic $acid-45\%$ Acetonitrile, and mobile phase B, comprising $2\%$ aqueous acetic acid, and delivered at a flow rate of 1mL/min as follows: 0-18 min, $50-100\%$ A; 18-20 min, $100-50\%$ A; 20-22 min, $50\%$ A. The UV detection wavelength was set at 355 nm. The limit of detection (LOD) for rutin standard compound was 20 ng/mL. And, the higher content of rutin in the extracts was obtained by $80^{\circ}C$ reflex extraction for 120 min. from plants of buckwheat using ethanol.

Analysis and Risk Assessment of Aflatoxin M1 in Infant Formula (분유 중 아플라톡신 M1 분석 및 위해평가)

  • Kang, YoungWoon;Song, Jeong-Eon;Suh, Junghyuck;Park, Sung Kug;Kim, Meehye
    • Korean Journal of Food Science and Technology
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    • v.45 no.2
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    • pp.235-240
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    • 2013
  • To analyze aflatoxin $M_1$ ($AFM_1$), we dissolved infant formula in warm water and cleaned it by using an immunoaffinity column (IAC). The amount of $AFM_1$ was determined by high-performance liquid chromatography coupled with fluorescence detection. $AFM_1$ was detected in 281 of 439 samples. Thus, the detection rate of $AFM_1$ was 64.0%. The average concentration of $AFM_1$ in positive samples was 2.6 ng/kg (of prepared formula). The estimated daily intake (EDI) of $AFM_1$ through infant formula was 0.087-0.646 ng/kg body weight/day and the additional number of cases of liver cancer associated with exposure to $AFM_1$ would be 0.003-0.020 cancer cases/1,000,000. Because there is less than 1 cancer case/1,000,000 per year, the exposure to $AFM_1$ through infant formula in Korea is considered to be an unlikely human health concern.

Evaluation of Tar Dyes Used in Commercial Foods (식품 중 합성첨가물 사용실태 조사 연구 -타르색소 중심으로-)

  • 윤미혜;김국주;김정임;황선일;문수경;정은주;김재관
    • Journal of Food Hygiene and Safety
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    • v.15 no.2
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    • pp.108-113
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    • 2000
  • This study was carried out to propose a simple method for the extraction of seven tar dyes such as tartrazine, sunset yellow FCF, amaranth, erythrosine, allura red, brilliant blue FCF and indigo carmine using aminopropyl amine cartridge and to determine the content of the dyes in candies, soft drinks, ice bars and okchuns produced in Korea. The tar dyes were simultaneously analyzed by reverse phase high performance liquid chromatography(HPLC). The recovery rates of the dyes ranged from 65.8% to 99.6%. The contents of the dyes in candies, soft drinks, ice bars and octhuns were N.D.∼50.1 mg/kg, N.D.∼49.9 mg/kg, N.D.∼56.0 mg/kg and N.D.∼867.3 mg/kg, respectively. The types of the dyes used most frequently for candies, soft drinks and ice bars were tartrazine, brilliant blue and amaranth, respectively. Of the samples, tartrazine was used frequently, and indigo carmine was not used at all.

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Analysis of Benzo[a]pyrene Content and Risk Assessment (훈제식육식품 중 벤조피렌 함량 분석 및 안전성 평가)

  • Cho, Hyoun-Kyoung;Kim, Mee-Hye;Park, Sung-Kug;Shin, Han-Seung
    • Food Science of Animal Resources
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    • v.31 no.6
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    • pp.960-965
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    • 2011
  • The content of benzo[a]pyrene from 69 smoked meat products commonly consumed in Korean food market was analysed with high performance liquid chromatography. Smoked meat products including smoked chicken, pork, turkey and duck were saponified, extracted and cleaned up to analyze the benzo[a]pyrene content. As a result of analysis from smoked meat products, the mean benzo[a]pyrene content was 0.42 ${\mu}g$/kg and the highest content of benzo[a]pyrene was 2.87 ${\mu}g$/kg detected in smoked chicken product. All somked meat products contained benzo[a]pyrene below the limit regulated by Korean Food and Drug Administration (KFDA). Exposure assessment of benzo[a]pyrene from smoked meat products ingestion was calculated by using National Health and Nutrition Survey (NHNS). The estimated lifetime average daily intake of benzo[a]pyrene was 0.187 ng/kg bw/d. Margin of exposure of benzo[a]pyrene was ranged from 1,657,754 to 3,957,219.

Hypoallergenic and Physicochemical Properties of the A2 β-Casein Fractionof Goat Milk

  • Jung, Tae-Hwan;Hwang, Hyo-Jeong;Yun, Sung-Seob;Lee, Won-Jae;Kim, Jin-Wook;Ahn, Ji-Yun;Jeon, Woo-Min;Han, Kyoung-Sik
    • Food Science of Animal Resources
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    • v.37 no.6
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    • pp.940-947
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    • 2017
  • Goat milk has a protein composition similar to that of breast milk and contains abundant nutrients, but its use in functional foods is rather limited in comparison to milk from other sources. The aim of this study was to prepare a goat A2 ${\beta}$-casein fraction with improved digestibility and hypoallergenic properties. We investigated the optimal conditions for the separation of A2 ${\beta}$-casein fraction from goat milk by pH adjustment to pH 4.4 and treating the casein suspension with calcium chloride (0.05 M for 1 h at $25^{\circ}C$). Selective reduction of ${\beta}$- lactoglobulin and ${\alpha}_s$-casein was confirmed using sodium dodecyl sulphate-polyacrylamide gel electrophoresis and reverse-phase high-performance liquid chromatography. The hypoallergenic property of A2 ${\beta}$-casein fraction was examined by measuring the release of histamine and tumor necrosis factor alpha from HMC-1 human mast cells exposed to different proteins, including A2 ${\beta}$-casein fraction. There was no significant difference in levels of both indicators between A2 ${\beta}$-casein treatment and the control (no protein treatment). The A2 ${\beta}$-casein fraction is abundant in essential amino acids, especially, branched-chain amino acids (leucine, valine, and isoleucine). The physicochemical properties of A2 ${\beta}$-casein fraction, including protein solubility and viscosity, are similar to those of bovine whole casein which is widely used as a protein source in various foods. Therefore, the goat A2 ${\beta}$-casein fraction may be useful as a food material with good digestibility and hypoallergenic properties for infants, the elderly, and people with metabolic disorders.

Determination of Preservatives in Pharmaceuticals and Personal Care Products (의약품 및 개인위생·생활용품 중 보존제 함유량 분석)

  • Kim, Boyoung;Lee, Joohee;Kim, Seonyeob;Lee, Eunji;Choi, Chorong;Kho, Younglim
    • Journal of Environmental Health Sciences
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    • v.42 no.1
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    • pp.53-60
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    • 2016
  • Objectives: Preservatives are commonly used in pharmaceuticals, cosmetics and other products to extend the expiration date and prevent the growth of microorganisms. Preservatives are generally effective in controlling mold and inhibiting yeast growth, and against a wide range of bacterial attacks as well. They also adversely affect the quality of sperm and cause precocious puberty in children. This study was performed to analyze seven preservatives used in pharmaceuticals and personal care products. Methods: Five kinds of pharmaceuticals and personal care products (PPCPs) were examined for analysis with a high performance liquid chromatography-diode array detector. Each sample was homogenized and the targeted compounds were extracted with methanol. The suspended particulate was removed by syringe filter. Next, the sample was injected into an HPLC system. The separation of the seven preservatives was achieved with a C18 column and gradient mode. The accuracies were between 73% and 120% and precision was lower than 11.58% (RSD). Results: All of the calibration curves showed good linearity with a coefficient of determination ($r^2$) over 0.999. Among the PPCP samples, the detection rate of preservatives was 32.5% for pharmaceuticals, 44.8% for toothpaste, 76.9% for mouthwash, 40.0% for body lotion and 56.0% for wet tissues. The average concentrations of the preservatives in PPCPs were BA 1141.0 mg/kg, MP 709.8 mg/kg, EP 624.9 mg/kg, PP 216.9 mg/kg, BP 167.8 mg/kg, and TCS 538.2 mg/kg. The most frequently detected preservatives in pharmaceuticals and personal care products were BA, MP and PP. The concentrations of preservatives exceeded Korean regulatory standards in 11 samples of medicines, three of mouthwash and two of body lotion. Conclusion: We found that most of the PPCP samples contained various preservatives. It is necessary to identify which preservatives were used and to determine the level of preservatives in PPCPs and to assess the health risk to susceptible populations such as children.

Synthesis and Characterization of Structured Lipids from Evening Primrose Seeds Oil and Rice Bran Oil (달맞이꽃 종자유와 미강유로부터 효소적 합성한 재구성 지질의 이화학적 특성 분석)

  • Kim, Hyo-Jin;Lee, Kyung-Su;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1156-1164
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    • 2010
  • Structured lipids (SLs) were synthesized by enzymatic interesterification with evening primrose oil (EPO) and rice bran oil (RBO) in a batch-type reactor. The interesterification was performed using a water shaker for 24 hr at $55^{\circ}C$. Mixing speed was set at 200 rpm and Lipozyme RM IM (immobilized lipase from Rhizomucor miehei, 10% by weight of total substrates) was used as a biocatalyst. Rice bran oil and evening primrose oil were interesterified with various molar ratios (RBO : EPO, 1:3, 1:4, and 1:5 mol/mol). Reversed-phase high performance liquid chromatography connected with evaporative light-scattering detector was performed to separate the triacylglycerol (TAG) species of SLs. In the fatty acid analysis, $\gamma$-linolenic acid (7.9 mol%), linoleic acid (67.3 mol%) and oleic acid (13.2 mol%) were the most abundant fatty acids in the SLs. During 24 hr reaction, most of the reaction occurred within 3 hr. TAG compositions, tocopherols and phytosterols were also analyzed. In the TAG species analysis, LLL (ECN=42, L=linoleic acid) dramatically decreased when the reaction time increased.

Development of Method for Analysis of Four Sulfonylurea Pesticides, Rimsulfuron, Ethametsulfuron-methyl, Tribenuron-methyl, Chlorimuron-ethyl Residues by High-Performance Liquid Chromatography with Diode-Array Detection (HPLC/DAD를 이용한 림술푸론, 에타메트설푸론메틸, 트리베누론메칠, 클로리무론에칠 4종 성분의 잔류농약 분석법 개발)

  • Koo, Yun-Chang;Yang, Sung-Yong;Wang, Zeng;An, Eun-Mi;Heo, Kyoung;Kim, Hyeng-Kook;Shin, Han-Seung;Lee, Jin-Won;Lee, Kwang-Won
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1231-1235
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    • 2010
  • The method for residue analysis of four sulfonylurea pesticides, rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl and chlorimuron-ethyl was examined and analyzed by HPLC with ODS column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size) which was maintained at $35^{\circ}C$. Mobile phase consisted of solvent A (20 mM $KH_2PO_4$, pH 2.5) and solvent B (acetonitrile). Isocratic elution of the column with 45% solvent A and 55% solvent B at a flow rate of 1 mL/min resulted in retention times of 5.92, 6.54, 9.28, and 14.35 min for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. All injection volumes were $20\;{\mu}L$. The limit of quantitation was 0.02, 0.01, 0.001, and 0.004 mg/kg for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four sulfonylurea pesticides were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 86.12% to 116.26% and the standard deviations of all experiments were within 10%.

Residues of Ampicillin and Amoxicillin in Olive Flounder Paralichthys olivaceus Following Oral Administration (양식 넙치(Paralichthys olivaceus)에 경구투여한 Ampicillin 및 Amoxicillin의 어류체내 잔류량의 변화)

  • Son, Kwang-Tae;Jo, Mi-Ra;Oh, Eun-Gyoung;Mok, Jong-Soo;Kwon, Ji-Young;Lee, Tae-Seek;Song, Ki-Cheol;Kim, Poong-Ho;Lee, Hee-Jung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.44 no.5
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    • pp.464-469
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    • 2011
  • Residues of ampicillin and amoxicillin in the muscles of olive flounder Paralichthys olivaceus were investigated after oral doses of 20 mg/kg body weight/day of ampicillin and 40 mg/kg body weight/day of amoxicillin in a first examination and 40 mg/kg body weight/day of ampicillin and 80 mg/kg body weight/day of amoxicillin in a second examination for 5-6 days. The ranges of seawater temperatures in the $1^{st}$ and $2^{nd}$ examinations were $13.4-15.6^{\circ}C$ and $16.8-21.4^{\circ}C$, respectively. Ampicillin and amoxicillin concentrations were analyzed by high performance liquid chromatography (HPLC). The average recovery rates of ampicillin and amoxicillin in fish samples ranged from 84.8-95.2% and 100.8-103.8%, respectively. Residual concentrations in the olive flounder peaked on the $5^{th}$ day, with average concentrations of 0.075 mg/kg and 0.311 mg/kg in the $1^{st}$ examination, and 0.098 mg/kg and 0.630 mg/kg in the $2^{nd}$ examination for ampicillin and amoxicillin, respectively, with maximum concentrations in muscle. In the $1^{st}$ examination, ampicillin concentrations in olive flounder after withdrawals of 1 and 3 days were 0.041 mg/kg and 0.023 mg/kg, respectively, and amoxicillin concentrations after withdrawals of 1 day and 10 days were 0.172 mg/kg and 0.023 mg/kg, respectively. In the $2^{nd}$ examination, the ampicillin concentrations in olive flounder after withdrawals of 1 and 3 days were 0.041 mg/kg and 0.023 mg/kg, respectively, and amoxicillin concentration after withdrawals of 1 day and 10 days were 0.172 mg/kg and 0.023 mg/kg, respectively. We suggest that the recommended withdrawal periods should be 3 days for ampicillin and 10 days for amoxicillin in the olive flounder.

Residues of Fluoroquinolones in Olive Flounder (Paralichthys olivaceus) and Black Rockfish (Sebastes schlegell) Following Oral Administration (Fluoroquinolone계 항생제의 경구투여에 따른 양식넙치 및 조피볼락의 체내 잔류량의 변화)

  • Kim, Poog-Ho;Lee, Doo-Seog;Kim, Jin-Woo;Park, Mi-Seon;Kim, Dong-Soo;Jo, Mi-Ra
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.42 no.4
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    • pp.329-334
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    • 2009
  • The residues of fluoroquinolones in Olive flounder (Paralichthys olivaceus) and Black rockfish (Sebastes schlegeli) were investigated after oral doses of 20 mg/kg for 30 days. Blood samples were taken at 5 hours, 10 hours, 1 day, 2 days, 3 days, 5 days, 7 days, 9 days, 13 days, 20 days and 30 days after treatment. The concentrations of fluoroquinolones were detected by high performance liquid chromatography using a UV detector. The recovery rates of fluoroquinolones in fish samples ranged from 92.0-99.7%, 93.4-97.5% and 93.0-97.9% for treatment of 0.1, 0.5, and $1.0{\mu}g/g$, respectively. Ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were detected in the blood of the olive flounder at 10 hours, 10 hours, 1 day and 10 hours after treatment with $6.43{\mu}g/g$, $6.07{\mu}g/g$, $11.83{\mu}g/g$ and $11.02{\mu}g/g$ as maximum level, respectively. Ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were detected in the blood of black rockfish 1 day, 1 day, 1 day and 10 hours after treatment with $8.26{\mu}g/g$, $8.03{\mu}g/g$, $7.29{\mu}g/g$ and $9.38{\mu}g/g$ as maximum level, respectively. However, ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were not detected in olive flounder samples at 20, 30, 20 and 20 days after treatment in any experiments (