• Title/Summary/Keyword: extracted liquid

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Residue analysis of penicillines in livestock and marine products (국내 유통 축·수산물 중 페니실린계 동물용의약품에 대한 잔류실태조사)

  • Song, Ji-Young;Hu, Soo-Jung;Joo, Hyun-Jin;Kim, Mi-Ok;Hwang, Joung-Boon;Han, Yoon-Jung;Kwon, Yu-Jihn;Kang, Shin-Jung;Cho, Dae-Hyun
    • Analytical Science and Technology
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    • v.25 no.4
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    • pp.257-264
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    • 2012
  • Penicillins belong to the ${\beta}$-lactam class of antibiotics, and are frequently used in human and veterinary medicine. Despite the positive effects of these drugs, improper use of penicillins poses a potential health risk to consumers. This study has been undertaken to determinate multi-residues of penicillins, including amoxicillin, ampicillin, oxacillin, bezylpenicillin, cloxacillin, dicloxacillin, and nafcillin, using liquid chromatographic tandem mass spectrometer (LC-MS/MS). The developed method was validated for specificity, precision, recovery, and linearity in livestock and marine products. The analytes were extracted with 80% acetonitrile and clean-up by a single reversed-phase solid-phase extraction step. Six penicillins presented recoveries higher than 76% with the exception of Amoxicillin. Relative standard deviations (RSDs) were not more than 10%. The method was applied to 225 real samples. Benzylpenicillin was detected in 12 livestock products and 7 marine products. Amoxicillin, ampicillin, cloxacilllin, dicloxacillin, nafcillin and oxacillin were not detected. The detected levels were 0.001~0.009 mg/kg in livestock products excluding eggs and milk. In marine products, the detected levels were under 0.03 mg/kg. They were under the MRL levels. As monitoring results, it is identified to be safe but it is considered that safety management of antibiotics should continue by monitoring.

Determination of cyromazine residues in agricultural commodities using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Cyromazine의 잔류분석법)

  • Song, Lee-Seul;Kim, Young-Hak;Lee, Su-Jin;Hwang, Young-Sun;Kwon, Chan-Hyeok;Do, Jung-Ah;Oh, Jae-Ho;Im, Moo-Hyeog;Chang, Woo-Suk;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.202-208
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    • 2012
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.

Method Development for the Sample Preparation and Quantitative Analysis of Synthetic Colors in Foods (식품 중 식용타르색소의 시료별 전처리방법 확립 및 함량 분석)

  • Park, Sung-Kwan;Lee, Tal-Su;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.36 no.6
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    • pp.893-899
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    • 2004
  • Method for sample preparation and quantitative analysis of 19 permitted and non-permitted synthetic colors in foods was developed based on reversed-phase ion-pairing high performance liquid chromatography. For color extraction of samples, deionized water was added, and pH was appropriately adjusted with 1% ammonia water. Any undissolved matters were extracted with 50% ethanol or 70% methanol. Lipid in snacks was first removed using n-hexane with centrifugation, water was added to extract colors, followed by clean-up and concentration using Sep-Pak $C_{18}$ cartridge. Recovery efficiencies at known concentrations of 19 standard food colors spiked into foods were in 90.3-97.9% range far soft drink, 79.2-101.9% for candy, 84.1-103.4% for jelly, 86.4-100.8% for chewing gum, 83.5-103.4% for ice cream, and 78.5-95.6% for snack.

Effects of Dietary Radish Green and Spinach on Meat Quality and Lutein Accumulation in Broiler Tissue (사료 내 무청 및 시금치 급여가 육계의 조직 내 루테인 축적률 및 육질에 미치는 영향)

  • Kang, Geun-Ho;Kim, Sang-Ho;Kim, Ji-Hyuk;Kang, Hwan-Ku;Kim, Dong-Wook;Cho, Soo-Hyun;Seong, Pil-Nam;Park, Beom-Young;Ham, Jun-Sang;Kim, Dong-Hun
    • Food Science of Animal Resources
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    • v.31 no.1
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    • pp.86-91
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    • 2011
  • This experiment was conducted to investigate the effects of dietary supplementation with lutein-containing materials on meat quality and lutein accumulation in broiler tissue. Broilers were subjected to one of the following treatments: C, basal diet (BD); T1, BD + 2.223% lutein from spinach extracted by ethanol fermentation; T2, BD + 2% radish green powder; T3, BD + 0.61% spinach powder; and T4, BD + 1.83% spinach powder. The weight gain, feed intake, and feed conversion did not differ among treatments. An evaluation of the color of the chicken breast meat revealed that the CIE $L^*$ value of the control was significantly (p<0.05) lower than that of the other treatments, whereas T4 had a significantly (p<0.05) lower CIE $a^*$ value and a higher (p<0.05) CIE $b^*$ value than the other treatments. The lipid oxidation (thiobarbituric acid reaction substances, TBARS) value was not significant among treatments. The results of a high performance liquid chromatography analysis revealed that the lutein peak was present only in the T4 liver tissue. These results showed that spinach powder (T4) affected meat color (CIE $a^*$ and $b^*$) however, TBARS and lutein accumulation were not affected.

Introduction and Expression of PAP gene using Agrobacterium in Scrophularia buergeriana Miquel (Agrobacterium을 이용한 PAP 유전자의 현삼으로 도입 및 형질발현)

  • Yu, Chang-Yeon;Seong, Eun-Soo;Lim, Jung-Dae;Huang, Shan-Ai;Chae, Young-Am
    • Korean Journal of Medicinal Crop Science
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    • v.9 no.2
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    • pp.156-165
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    • 2001
  • Exogeneous application of pokeweed antiviral protein (PAP), a ribosomal-inacivating protein in the cell wall of Phytolacca americana (pokeweed) protects heterologous plants from viral and fungal infection. A cDNA clone of PAP introduced into Scrophularia buergeriana Miquel by thransformation with Agrobacterium tumefaciences. For plant transformation, explants were precultured on shoot induction medium without kanamycin for 2-5 day, and then they were cocultured with Agrobacterium for 10 minutes. The explants were placed on co culture medium in dark condition, $28^{\circ}C$ for 2days. After explants were washed in MS liquid medium, they were transferred into selection medium including kanamycin 50mg/L (MS salts+1mg/ l BAP+2mg/ l TDZ+0,2mg/ l NAA+MS vitamin+3% sucrose+0.8% agar, pH5.8). From PCR analysis, NPT II band was confirmed in transgenic plant genome and showed resistance against fungi in antifungal activity test. Micro assay to which protein extracted from transgenic line were added, revealed hyphae growth inhibition and no spore germination at high concentration. The characteristics of inhibited hyphae was represented transparent and thin. Expression of PAP in transgenic plants offers the possibility of developing resistance to viral and fungal infection.

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Antibacterial and Antimutagenic Effects of Sweetpotato Tips Extract (고구마 끝순 추출물의 항균 및 항돌연변이 효과)

  • Lee, Joon-Seol;Shin, Mee-Jin;Park, Yang-Kyun;Ahn, Young-Sup;Chung, Mi-Nam;Kim, Hag-Sin;Kim, Jeong-Mok
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.52 no.3
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    • pp.303-310
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    • 2007
  • Sweetpotato shoot tops (leaves, tips and petioles) are known to be very useful parts as vegetables because of their high nutritive values and great biomass yield. In this study, the phenolic compound contents, antibacterial activity, mutagenic activity, and antimutagenic activity were investigated in sweetpotato tips that were 10-15cm of shoot top including stems, petioles and tender leaves after sprout of storage roots. The study was done by extracting sweetpotato tips with 80% ethanol and the ethanol fraction was re-extracted with hexane, chloroform, ethyl acetate, butanol and water. In ethyl acetate and butanol fractions, total phenolic compounds contained 95. 6mg/g extract and 69.3 mg/g extract, respectively, The antibacterial activity was measured using the paper disk method with concentrations of 1, 2, 5 and 10 mg/disk of butanol and ethyl acetate fractions against L. monocytogenes and S. Typhimurium strains. Higher doses of solvent extracts showed the higher antibacterial activities. In addition, 5, 10 and 20 mg/mL of the extracts were tested to determine the antibacterial activity in liquid culture. The sweetpotato leaf extract by ethyl acetate showed 1 log reduction compared to control after 24 hrs on Listeria monocytogenes, but 20 mg/ml of butanol extract completely inhibited the growth of the pathogen after 12 hrs. The extracts from ethyl acetate or butanol on Salmonella Typhimurium did less than 1 log reduction during cultivation compared to control. The numbers of S. Typhimirium TA98 and TA100 revertant colonies were 29-33 and 159-188 CFU/plate, respectively, indicating that solvent extracts were no mutagenic activity. The antimutagenic test was performed by adding direct mutagen 2-NF and MMS, and butanol and ethyl acetate showed antimutagenic effect. Thus, this study showed that sweetpotato tips had high phenolic contents and both antimicrobiol and antimutagenic properties. Sweetpotato tips would be good nutritive source because of their high nutrient content without any toxicity in consuming.

Monitoring of Benzoic Acid, Sorbic Acid, and Propionic Acid in Spices (향신료에서 유래되는 안식향산, 소브산, 프로피온산의 함유량 조사)

  • Yun, Sang Soon;Lee, Sang Jin;Lim, Do Yeon;Lim, Ho Soo;Lee, Gunyoung;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.381-388
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    • 2017
  • In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.

Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증)

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Risk Analysis of Inorganic Arsenic in Foods (식품 중 무기비소의 위해 분석)

  • Yang, Seung-Hyun;Park, Ji-Su;Cho, Min-Ja;Choi, Hoon
    • Journal of Food Hygiene and Safety
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    • v.31 no.4
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    • pp.227-249
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    • 2016
  • Arsenic and its compounds vary in their toxicity according to the chemical forms. Inorganic arsenic is more toxic and known as carcinogen. The provisional tolerable weekly intake (PTWI) of $15{\mu}g/kg$ b.w./week established by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) has been withdrawn, while the EFSA panel suggested $BMDL_{0.1}$ $0.3{\sim}8{\mu}g/kg\;b.w./day$ for cancers of the lung, skin and bladder, as well as skin lesions. Rice, seaweed and beverages are known as food being rich in inorganic arsenic. As(III) is the major form of inorganic arsenic in rice and anaerobic paddy soils, while most of inorganic arsenic in seaweed is present as As(V). The inorganic arsenic in food was extracted with solvent such as distilled water, methanol, nitric acid and so on in heat-assisted condition or at room temperature. Arsenic speciation analysis was based on ion-exchange chromatography and high-performance liquid chromatography equipped with atomic absorption spectrometry and inductively coupled plasma mass spectrometry. However, there has been no harmonized and standardized method for inorganic arsenic analysis internationally. The inorganic arsenic exposure from food has been estimated to range of $0.13{\sim}0.7{\mu}g/kg$ bw/day for European, American and Australian, and $0.22{\sim}5{\mu}g/kg$ bw/day for Asian. The maximum level (ML) for inorganic arsenic in food has established by EU, China, Australia and New Zealand, but are under review in Korea. Until now, several studies have conducted for reduction of inorganic arsenic in food. Inorganic arsenic levels in rice and seaweed were reduced by more polishing and washing, boiling and washing, respectively. Further research for international harmonization of analytical method, monitoring and risk assessment will be needed to strengthen safety management of inorganic arsenic of foods in Korea.

Method Development for the Profiling Analysis of Endogenous Metabolites by Accurate-Mass Quadrupole Time-of-Flight(Q-TOF) LC/MS (LC/TOFMS를 이용한 생체시료의 내인성 대사체 분석법 개발)

  • Lee, In-Sun;Kim, Jin-Ho;Cho, Soo-Yeul;Shim, Sun-Bo;Park, Hye-Jin;Lee, Jin-Hee;Lee, Ji-Hyun;Hwang, In-Sun;Kim, Sung-Il;Lee, Jung-Hee;Cho, Su-Yeon;Choi, Don-Woong;Cho, Yang-Ha
    • Journal of Food Hygiene and Safety
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    • v.25 no.4
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    • pp.388-394
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    • 2010
  • Metabolomics aims at the comprehensive, qualitative and quantitative analysis of wide arrays of endogenous metabolites in biological samples. It has shown particular promise in the area of toxicology and drug development, functional genomics, system biology and clinical diagnosis. In this study, analytical technique of MS instrument with high resolution mass measurement, such as time-of-flight (TOF) was validated for the purpose of investigation of amino acids, sugars and fatty acids. Rat urine and serum samples were extracted by selected each solvent (50% acetonitrile, 100% acetonitrile, acetone, methanol, water, ether) extraction method. We determined the optimized liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) system and selected appropriated columns, mobile phases, fragment energy and collision energy, which could search 17 metabolites. The spectral data collected from LC/TOFMS were tested by ANOVA. Obtained with the use of LC/TOFMS technique, our results indicated that (1) MS and MS/MS parameters were optimized and most abundant product ion of each metabolite were selected to be monitorized; (2) with design of experiment analysis, methanol yielded the optimal extraction efficiency. Therefore, the results of this study are expected to be useful in the endogenous metabolite fields according to validated SOP for endogenous amino acids, sugars and fatty acids.