• Title/Summary/Keyword: liquid-liquid extraction

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Analysis and Safety Assessment of Antioxidants Migrated from Polyethylene and Polypropylene Food Packaging Materials into Food Simulants (폴리에틸렌 및 폴리프로필렌 기구·용기·포장 유래 산화방지제 분석 및 안전성평가)

  • Choi, Heeju;Choi, Jae Chun;Bae, In-Ae;Park, Se-Jong;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.424-433
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    • 2017
  • Antioxidants are used in the manufacturing of commercial food packages made of polyolefin plastic such as polyethylene and polypropylene for the purpose to delay the oxidation reaction of the polymer due to oxygen or traces of ozone in the atmosphere. Additives in plastics may be migrated from the packaging materials into foods, thereby presenting a potential health risk to the consumer. Therefore, it is necessary to determine migration level of antioxidants from food packaging materials to foodstuffs in order to take proactive management. In this study, we have developed a method for the analysis of 10 antioxidants, which are butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), Cyanox 2246, 425 and 1790, Irgafos 168, and Irganox 1010, 1330, 3114 and 1076, migrated from the food packaging materials into four food simulants for aqueous, acidic, alcoholic and fatty foods. The antioxidants were determined by reversed-phase high-performance liquid chromatograph-ultraviolet detector with 276 nm after solid-phase extraction with a hydrophilic-lipophilic balance (HLB) cartridge or dilution with isopropanol. The analytical method showed a good linearity of coefficient ($R^2{\geq}0.99$), limits of detection (0.11~0.41 mg/L), and limits of quantification (0.34~1.24 mg/L). The recoveries of antioxidants spiked to four food simulants ranged from 71.3% to 109.4%. The migrated antioxidants in this study were within the safety levels that resulted from the safety assessment by the estimated daily intake to the tolerable daily intake.

Simultaneous Determination of UV Absorbers Migrated from Polyethylene and Polypropylene Food Packaging Materials into Food Simulants by HPLC-UVD (HPLC-UVD를 이용한 폴리에틸렌, 폴리프로필렌 기구 및 용기·포장 유래 자외선흡수제 동시분석법)

  • Choi, Heeju;Choi, Jae Chun;Bae, In-Ae;Lee, Chanyong;Park, Se-Jong;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.434-442
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    • 2017
  • The UV light in sunlight breaks down the chemical bonds in a polyolefin polymer through a process called photodegradation, ultimately causing cracking, chalking, colour changes, and loss of physical properties such as impact strength, tensile strength, elongation, and others. UV absorbers are used to prevent or terminate the oxidation of plastics by UV light. They are receptive to UV radiation and dissipate the energy harmlessly as heat. Benzotriazoles and benzophenones are used mainly in polyolefins such as polyethylene and polypropylene. In this study, we have developed a method for the analysis of 12 UV absorbers, which are Uvinul 3000, Cyasorb UV 24, Uvinul 3040, Tinuvin 312 and P, Seesorb 202, Chimassorb 81, Tinuvin 329, 234, 326, 328 and 327, migrated from the food packaging materials into four food simulants for aqueous, acidic, alcoholic and fatty foods. The UV absorbers in food simulants were determined by reversed-phase high performance liquid chromatograph-ultraviolet detector with 310 nm after solid-phase extraction with a hydrophilic-lipophilic balance (HLB) cartridge or dilution with isopropanol. The analytical method showed a good linearity of coefficient ($R^2{\geq}0.99$), limits of detection (0.049~0.370 mg/L), and limits of quantification (0.149~1.120 mg/L). The recoveries of UV absorbers spiked to four food simulants ranged from 70.05% to 110.13%. The developed method would be used as a reliable tool to determine concentrations of the migrated UV absorbers.

Occurrence and Distribution of Selected Veterinary Antibiotics in Soils, Sediments and Water Adjacent to a Cattle Manure Composting Facility in Korea (국내 우분 퇴비화 시설 인근 농경지 및 수계 중 Tetracycline 및 Sulfonamide 계열 항생물질의 분포특성)

  • Lim, Jung-Eun;Kim, Sung-Chul;Lee, Hyeon-Yong;Kwon, Oh-Kyung;Yang, Jae-E.;Ok, Yong-Sik
    • Journal of Korean Society of Environmental Engineers
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    • v.31 no.10
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    • pp.845-854
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    • 2009
  • There has been increased concern regarding the release of antibiotics to different environmental compartments due to the possibility of the development of antibiotic resistant bacteria. However, limited information is available regarding the occurrence, fate, and transport of antibiotics in Korea in both the aqueous phase and in solid phases such as sediment and soil. Therefore, this study was conducted to monitor the concentration of released antibiotics in surface water, sediment, and soil adjacent to a cattle manure composting facility in Korea. Specifically, the following six antibiotics were monitored: tetracycline (TC), chlortetracycline (CTC), oxytetracycline (OTC), sulfamethazine (SMT), sulfamethoxazole (SMX), and sulfathiazole (STZ). To extract and quantify the antibiotics from different environmental compartments, solid phase extraction (SPE) and high performance liquid chromatography mass spectrometry (HPLC/MS) techniques were adopted. The concentration of the six antibiotics ranged from below the detection limit (BDL) to 0.71 ${\mu}g$/L in surface water, from BDL to 27.61 ${\mu}g$/L in sediment, and from 0.12 to 157.33 ${\mu}g$/L in soil. In addition, higher concentrations of antibiotics were observed in surface water and sediment at locations closer to the composting facility indicating that composting is the source of the antibiotics found in the environment. Furthermore, higher concentrations of antibiotics were observed in the solid phase (sediment and soil) than the aqueous phase. These findings indicate that the possibility of antibiotic resistant bacteria is increased because such bacteria are more stable in the solid phase. Overall, longterm monitoring of the aqueous phase and solid phase is necessary to gain a better understanding of the impact of antibiotics from source on the environment in Korea.

Antioxidative Effects of Inula britannica var. chinensis Flower Extracts According to the flowering period and species of Inula britannica var. chinensis (금불초 종(種) 및 개화시기에 따른 금불초 꽃 추출물의 항산화 효능)

  • Kwon, Soon Sik;Jeon, So Ha;Jeon, Ji Min;Cheon, Jong Woo;Park, Soo Nam
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.39 no.3
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    • pp.195-203
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    • 2013
  • In this study, antioxidative effects of the extracts of different species and flowering periods of Inula britannica were investigated. According to the free radical (1,1-diphenyl-2-picrylhydrazyl, DPPH) scavenging activity of the extracts, The I. britannica var. chinensis flower extract (500 ${\mu}g/mL$) was measured in a 79.89% free radical scavenging activity, but the flower extracts of similar species (I. britannica var. linariaefolia Regel, I. britannica var. ramosa, I. salicina var. asiatica) did not show any effect on the free radical scavenging activity. The effects of the free radical scavenging activity of I. britannica var. chinensis flower extracts were exhibited in the order of full bloom (93.68%), bud (43.28%), and fallen blossom (14.11%). Next, we established optimum condition of extract solvent, temperature, extraction time. The extract from ethanol at $60^{\circ}C$ showed the most free radical scavenging activity among other conditions and extraction time not relevant in free radical scavenging activity. The protective effects of the extract of I. britannica var. chinensis flower on the photohemolysis of human erythrocytes by using rose bengal were increased in a concentration-dependent manner (5 ~ 50 ${\mu}g/mL$). In particular, the extract in 50 ${\mu}g/mL$ concentration exhibited better protective activity (${\tau}_{50}$ = 116.1 min) than (+)-${\alpha}$-tocopherol (${\tau}_{50}$ = 73.44 min), which is a known lipophilic antioxidant. Principle component of I. britannica var. chinensis flower was identified as quercetin of flavonoids by high-performance liquid chromatography (HPLC). These results indicate that the extract of I. britannica var. chinensis flower can function as antioxidants in biological systems, particularly skin exposed to UV radiation by scavenging free radical and $^1O_2$, and protect cellular membranes against ROS. It is concluded that the antioxidative effects of the extract of I. britannica var. chinensis flower could be applicable to functional cosmetics.

Dietary Fiber and β-Glucan Contents of Sparassis crispa Fruit Fermented with Lactobacillus brevis and Monascus pilosus (유산균 및 홍국균 발효 꽃송이버섯 추출물과 잔사의 식이섬유와 베타 글루칸의 함량)

  • Lim, Chang Wan;Kang, Kyoung Kyu;Yoo, Young-Bok;Kim, Byung Hee;Bae, Song-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.12
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    • pp.1740-1746
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    • 2012
  • Sparassis (S.) crispa is an edible mushroom abundant in dietary fiber and ${\beta}$-glucan. The aim of this study was to prepare extracts and residues of the fruit bodies of S. crispa fermented with Lactobacillus (L.) brevis and Monascus (M.) pilosus and to measure the remaining dietary fiber and ${\beta}$-glucan. Dried powder of S. crispa containing 64.4 g/100 g total dietary fiber (2.6 g/100 g soluble and 61.8 g/100 g insoluble dietary fibers) and 24.0 g/100 g ${\beta}$-glucan was used as the starting material for the extraction. Raw and fermented S. crispa were extracted with hot water and three kinds of aqueous ethanol (50, 70, and 90%, v/v), respectively. A hot water extract from S. crispa fermented with M. pilosus had greater soluble dietary fiber content (19.3 g/100 g) than that from raw S. crispa with 14.6 g/100 g soluble dietary fiber or that from L. brevis-fermented S. crispa with 8.2 g/100 g soluble dietary fiber. The yield of the extract was 16.6% of intial weight of dried S. crispa. After hot water extraction of S. crispa fermented with M. pilosus, residues containing 90.5 g/100 g total dietary fiber (1.3 g/100 g soluble and 89.2 g/100 g insoluble dietary fibers) were obtained, and the yield was 69.6% of intial weight of dried S. crispa. The residue (31.0 g/100 g) contained more ${\beta}$-glucan than raw S. crispa or M. pilosus-fermented S. crispa (24.4 g/100 g). The resulting hot water extract and residue from S. crispa fermented with M. pilosus would be suitable for use in preparing liquid and powdered health functional foods, respectively.

Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

Multi-residue Pesticide Analysis in Cereal using Modified QuEChERS Samloe Preparation Method (곡물류 중 잔류농약 다성분 분석을 위한 개선된 QuEChERS 시료 정제법의 개발)

  • Yang, In-Cheol;Hong, Su-Myeong;Kwon, Hye-Young;Kim, Taek-Kyum;Kim, Doo-Ho
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.314-334
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    • 2013
  • This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

Development and Validation of Analytical Method for Nitroxoline in Chicken Using HPLC-PDA (HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Eun;Kim, Jae-Young;Kang, Ilhyun;Lee, Sang-Mok;Do, Jung-Ah;Oh, Jae-Ho;Chang, Moon-Ik;Hong, Jin-Hwan
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.70-77
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    • 2013
  • BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

Establishment of Biotin Analysis by LC-MS/MS Method in Infant Milk Formulas (LC-MS/MS를 이용한 조제유류 중 비오틴 함량 분석법 연구)

  • Shin, Yong Woon;Lee, Hwa Jung;Ham, Hyeon Suk;Shin, Sung Cheol;Kang, Yoon Jung;Hwang, Kyung Mi;Kwon, Yong Kwan;Seo, Il Won;Oh, Jae Myoung;Koo, Yong Eui
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.327-334
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    • 2016
  • This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

Characterization of Antibacterial Compounds from Bacillus polyfermenticus CJ6 and Its Growth Inhibition Effect on Food-Borne Pathogens (Bacillus polyfermenticus CJ6가 생산하는 항세균 물질의 특성 및 병원성 식중독 미생물의 성장 억제 효과)

  • Jung, Ji-Hye;Chang, Hae-Choon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.6
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    • pp.903-911
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    • 2011
  • In this study, Bacillus polyfermenticus CJ6 harboring antibacterial activity was isolated from meju. The antibacterial activity of Bacillus polyfermenticus CJ6 was stable in the pH range of 3.0~9.0, but it disappeared after culture at $70^{\circ}C$ for 24 hr. Antibacterial activity was inactivated by proteinase K, protease, and ${\alpha}$-chymotrypsin, indicating its proteinaceous nature. The growth inhibitory effects of B. polyfermenticus CJ6 culture on food-borne pathogens such as Staphylococcus aureus, Salmonella Typhi, Listeria monocytogenes, and Escherichia coli O157:H7 were examined in this study. Approximately 6~6.2 log CFU/mL of each pathogen was co-cultured with B. polyfermenticus CJ6 in a 50 mL culture volume for 24 hr. Growth of S. aureus and L. monocytogenes was completely inhibited after 3 hr of incubation. Growth of S. Typhi and E. coli O157:H7 was also completely inhibited after 6 hr of incubation. The antibacterial compounds from B. polyfermenticus CJ6 were purified by solid phase extraction (C18 Sep-pak cartridge), recycling preparative HPLC, and analytical HPLC. Ultra-high performance liquid chromatography and electrospray ionization tandem mass spectrometry analysis were used to identify the purified antibacterial compounds, which were confirmed to be five peptides (757.4153 Da, 750.3444 Da, 1024.5282 Da, 1123.6083 Da, and 1617.8170 Da).