• Title/Summary/Keyword: ultra-performance liquid chromatography

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Analysis of Zearalenone Contamination in Cereal-Based Products Using High Performance Liquid Chromatography-Fluorescence Detector and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry (곡류가공품 중 제랄레논 오염도 조사)

  • Jang, Mi-Ran;Lee, Chang-Hee;Choi, In-Sun;Shin, Choon-Shik;Kim, Jin-Hee;Jang, Young-Mi;Kim, Dong-Sul;Ahn, Dong-Hyun
    • Korean Journal of Food Science and Technology
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    • v.43 no.2
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    • pp.224-229
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    • 2011
  • Zearalenone (ZEA) is an estrogenic mycotoxin mainly produced by Fusarium graminerum, a species which colonizes a wide variety of cereals, including wheat, barley and processed products. A survey of ZEA contamination was conducted on 141 dried confectioneries, 59 breads and rice cakes, 135 noodles and 101 other products, for a total of 432 commercial samples. Samples were analyzed by high performance liquid chromatography with fluorescence detection (HPLC-FLD) after immunoaffinity clean-up and was confirmed by liquid chromatography tandem mass spectrometry (LCMS/MS). The limits of detection and quantification were 2.0 and $6.0{\mu}g/kg$, respectively. The recovery ranged from 80.2% to 98.4% in the cereal based product. ZEA was detected in 38 samples (8.8% incidence), including 3 snack, 2 biscuit and 33 other cereal products. The ZEA contamination levels were in the range of $5.38-53.76{\mu}g/kg$. Finally, LC-MS/MS analysis of the contaminated samples was conducted to confirm the detected ZEA, and all 38 samples showing ZEA by HPLC-FLD were confirmed by LC-MS/MS.

A Survey of Zearalenone in Beans Using High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FLD) and Ultra Performance Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) (HPLC-FLD 및 LC-MS/MS에 의한 두류 중 제랄레논 오염실태 조사)

  • Jang, Mi-Ran;Lee, Chang-Hui;Lee, Hyo-Jeong;Kim, Ji-Yeon;Son, Sang-Hyeok;Sin, Chun-Sik;Kim, So-Hui;Kim, Dae-Byeong
    • Korean Journal of Food Science and Technology
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    • v.40 no.3
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    • pp.354-359
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    • 2008
  • A survey for zearalenone contamination was conducted on 27 soy bean samples, 27 red bean samples, 16 black bean samples, 19 seoritae samples, 14 seomoktae samples, for a total of 127 commercial Korean samples. Zearalenone was quantified by the immunoaffinity column clean-up method with high performance liquid chromatography-fluorescence detection (HPLC-FLD), and was confirmed by liquid chromatography tandem mass spectrometry(LC-MS/MS). The limits of detection and quantification were $2.0{\mu}g/kg$ and $6.0{\mu}g/kg$, respectively. The recovery in the beans ranged from 82.2 to 98.4%. According to HPLC-FLD, zearalenone was detected in 13 samples (10.2% incidence), including 1 soybean and 12 red bean samples. The zearalenone contamination levels were in the range of 8.01${\sim}38.98{\mu}g/kg$. Finally, LC-MS/MS analysis was conducted in the contaminated samples to verify the results of HPLC-FLD. The LC-MS/MS results confirmed the presence of zearalenone in all 13 samples. The contamination level was lower than that of EU, which is below $100{\mu}g/kg$ for raw grains.

Comparison of medical history based diagnosis and urine test using ultra-performance liquid chromatography-tandem mass spectrometry in drug overdose (약물중독 환자에서 병력 기반 진단과 요 고성능 액체색층분석 탄뎀 질량 분광분석의 비교)

  • Lee, Ja-Young;Cha, Kyungman;Jeong, Won Jung;Kim, Hyung Min;So, Byung Hak
    • Journal of The Korean Society of Clinical Toxicology
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    • v.20 no.1
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    • pp.1-7
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    • 2022
  • Purpose: In patients with acute drug overdose, identification of drugs ingested is crucial to make a precise diagnosis. In most cases, the diagnoses are made on the medical history and physical examination findings. This study was undertaken to determine the concordance of diagnosis made on the basis of patient history by comparing it with urine toxicology analysis. Methods: This was a retrospective study of drug intoxicated patients over 18 years old who presented to the emergency center from 2017 to 2019. Specimens from urine were tested using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-TMS). The test results were compared with information obtained from patients. Diagnostic concordances for drug detection in intoxicated patients were calculated. Logistic regression analysis was used to examine the association between clinical characteristics and diagnostic discrepancy. Results: Totally, 370 patients were included in the analysis. Overall, 66 types of drugs were detected by UPLC-TMS. The drugs detected most frequently were zolpidem (104, 27.8%), citalopram (70, 18.7%), and paracetamol (66, 17.6%). The mean diagnostic concordance of patients was 52.7%. There were statistically significant diagnostic discrepancies in patients with underlying depression and patients intoxicated with multiple types of drugs. Conclusion: In ED patients with acute drug overdose, the diagnoses made on history alone were often inaccurate. It is essential to perform urine toxicology tests such as UPLC-TMS as a confirmatory instrument to improve accuracy in evaluating patients with drug intoxication.

Phytoecdysones from the Roots of Achyranthes japonica Nakai and their Anti-atopy Activity (우슬의 뿌리로부터 Phytoecdysones의 분리와 항 아토피 효과)

  • Kim, Ki Ohk;Ku, Chang-Sub;Kim, Min-Jin;Park, Yhun Jung;Ryu, Hyung Won;Song, Hyuk-Hwan;Kim, Jung Hee;Oh, Sei-Ryang
    • Journal of Applied Biological Chemistry
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    • v.58 no.1
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    • pp.13-19
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    • 2015
  • The roots of Achyranthes japonica Nakai were extracted with 100% aqueous and concentrated subfraction was separated with ultra-performance liquid chromatography-based activity profiling. Three compounds were isolated from the subfraction 5 through the repeated prep- high performance liquid chromatography column chromatography. According to the results of physico-chemical and spectroscopic data including NMR and MS, the chemical structures of the compounds were determined as ecdysterone (1), 25S-inokosterone (2), and 25R-inokosterone (3). Three phytoecdysones were showed weak inhibitory activity for thymus and activation-regulated chemokine expression levels in tumor necrosis factor (TNF)-${\alpha}$ plus IFN-${\gamma}$ induced HaCaT cells, respectively. However, those compounds 1-3 were exhibited the most potent inhibition (80-95% at $200{\mu}g/mL$) against TNF-${\alpha}$ expression levels in A23187 plus phorbol-myrisrate acetate-induced RBL-2H3 cells. As result, 100% aqueous extract of A. japonica has an excellent anti-atopy activity. It could be used to a large range of functional anti-atopy cosmetics.

The Effect of pH and Temperature on Lysozyme Separation in Ion-exchange Chromatography (이온교환크로마토그래피에서 라이소자임 분리에 미치는 pH와 온도 영향)

  • Ko, Kwan-Young;Kim, In-Ho
    • Korean Chemical Engineering Research
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    • v.52 no.1
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    • pp.98-105
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    • 2014
  • Lysozyme amounts to 0.3% in egg white and functions as an agent of cell lysis and activator of tissue reconstruction. Ion exchange chromatography is the most useful method of separation among affinity chromatography, ion exchange chromatography, and ultra-filtration. The aim of present study is to find the optimum pH and temperature for the separation of lysozyme in egg white within cation exchange gel filled glass column. And we compared results of experiments with those of simulations. Phosphate buffer was used, and pH and temperature were varied as 5~7 and $25{\sim}40^{\circ}C$ respectively. RP-HPLC was the tool for the retention time identification and quantitative analysis of lysozyme. OriginPro 8 measured the peak area of lysozyme chromatogram and quantified the eluted lysozyme. Largest amount of lysozyme was separated under the conditions of pH 5 and T $25^{\circ}C$.

Comparison of Traditional and Commercial Vinegars Based on Metabolite Profiling and Antioxidant Activity

  • Jang, Yu Kyung;Lee, Mee Youn;Kim, Hyang Yeon;Lee, Sarah;Yeo, Soo Hwan;Baek, Seong Yeol;Lee, Choong Hwan
    • Journal of Microbiology and Biotechnology
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    • v.25 no.2
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    • pp.217-226
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    • 2015
  • Metabolite profiles of seven commercial vinegars and two traditional vinegars were performed by gas chromatography time-of-flight mass spectrometry with multivariate statistical analysis. During alcohol fermentation, yeast, nuruk, and koji were used as sugars for nutrients and as fermentation substrates. Commercial and traditional vinegars were significantly separated in the principal component analysis and orthogonal partial least square discriminant analysis. Six sugars and sugar alcohols, three organic acids, and two other components were selected as different metabolites. Target analysis by ultra-performance liquid chromatography quadruple-time-of-flight mass spectrometry and liquid chromatography-ion trap-mass spectrometry/mass spectrometry were used to detect several metabolites having antioxidant activity, such as cyanidin-3-xylosylrutinoside, cyanidin-3-rutinoside, and quercetin, which were mainly detected in Rural Korean Black raspberry vinegar (RKB). These metabolites contributed to the highest antioxidant activity measured in RKB among the nine vinegars. This study revealed that MS-based metabolite profiling was useful in helping to understand the metabolite differences between commercial and traditional vinegars and to evaluate the association between active compounds of vinegar and antioxidant activity.

Water-Soluble Vitamins Contents in Seafood-Based Dishes (수산물 조리 식품에 함유된 수용성 비타민 함량)

  • Kim, Naeun;Kim, Younghwa
    • The Korean Journal of Food And Nutrition
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    • v.33 no.4
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    • pp.390-398
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    • 2020
  • The purpose of this study was to determine the contents of water-soluble vitamins B1 (thiamine), B2 (riboflavin), B3 (niacin) and B12 (cyanocobalamin) in seafood-based dishes by using the high-performance liquid chromatography with the ultra violet and fluorescence detector. The vitamin B1, B2, B3 and B12 contents were analyzed in 29 seafood-based dishes. The method validation was performed on the method to determine the linearity, accuracy, limits of quantification, limits of detection and precision for vitamin B1, B2, B3 and B12. An excellent linearity range (R2=0.999~1.000) in the calibration curve for the water-soluble vitamins was observed. All analytical methods for the water-soluble vitamins showed the acceptable accuracy (89.4~119.7% recovery) and the precision (0.6~4.8% repeatability and 1.0~4.2% reproducibility). The highest content of vitamin B1 was 2.646 mg/100 g in the kkongchi-jorim, and the highest contents of vitamin B2, B3 and B12 were 0.370 mg/100 g, 10.971 mg/100 g, and 17.193 ㎍/100 g, respectively, in the kkongchi-gui. Our results provide reliable data on the contents of the water-soluble vitamins of seafood-based dishes in Korea.

Identification of Factors Regulating Escherichia coli 2,3-Butanediol Production by Continuous Culture and Metabolic Flux Analysis

  • Lu, Mingshou;Lee, Soo-Jin;Kim, Bo-Rim;Park, Chang-Hun;Oh, Min-Kyu;Park, Kyung-Moon;Lee, Sang-Yup;Lee, Jin-Won
    • Journal of Microbiology and Biotechnology
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    • v.22 no.5
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    • pp.659-667
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    • 2012
  • 2,3-Butanediol (2,3-BDO) is an organic compound with a wide range of industrial applications. Although Escherichia coli is often used for the production of organic compounds, the wild-type E. coli does not contain two essential genes in the 2,3-BDO biosynthesis pathway, and cannot ferment 2,3-BDO. Therefore, a 2,3-BDO biosynthesis mutant strain of Escherichia coli was constructed and cultured. To determine the optimum culture factors for 2,3-BDO production, experiments were conducted under different culture environments ranging from strongly acidic to neutral pH. The extracellular metabolite profiles were obtained using high-performance liquid chromatography (HPLC), and the intracellular metabolite profiles were analyzed by ultra-performance liquid chromatography and quadruple time-of-flight mass spectrometry (UPLC/Q-TOF-MS). Metabolic flux analysis (MFA) was used to integrate these profiles. The metabolite profiles showed that 2,3-BDO production favors an acidic environment (pH 5), whereas cell mass favors a neutral environment. Furthermore, when the pH of the culture fell below 5, both the cell growth and 2,3-BDO production were inhibited.

Preservatives in Domestic and Imported Children's Clay Products (국내 시판 어린이 점토제품 중 보존제 함유량 조사)

  • Jung, Sun Hye;Heo, Jin Yeong;Oh, Ji Hee;Park, Na-Youn;Kho, Younglim
    • Journal of Environmental Health Sciences
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    • v.48 no.1
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    • pp.36-43
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    • 2022
  • Background: Preservatives are used to prevent product deterioration in modeling clay. Parabens, a representative preservative, have been found to be endocrine disruptors and cause skin irritation and allergic reactions. Isothiazolinone preservatives can be irritating to the skin, respiratory tract, and eyes. Thorough investigation and regulation of clay are necessary because clay is marketed to children, who are more sensitive to the toxic effect of chemicals. Objectives: In this study, the presence of 16 preservatives was analyzed in modeling clay and the results were compared with current standards. Methods: A total of 200 samples were collected from 28 children's clay products sold in South Korea (13 from Korea and 15 imported from overseas). Twelve preservatives, such as parabens, were analyzed using high-performance liquid chromatography (HPLC). Isothiazolinone preservatives (chloromethylisothiazolinone; CMIT, methylisothiazolinone; MIT, octylisothiazolinone; OIT, and benzisothiazolinone; BIT) were analyzed using ultra performance liquid chromatography-tandem mass spectrometery (UPLC-MS/MS). Results: Dehydroacetic acid (DHA) was detected the most in the clays at 51.50% (103 cases) detection; 38 cases (median 190.42 ㎍/g) in Korean products and 65 cases (median 169.62 ㎍/g) in Chinese products. CMIT, which is prohibited in Korea, was detected in 14 (median 16.28 ㎍/g) Chinese products. OIT, which has a chemical structure similar to CMIT was found in 28 (median 68.38 ㎍/g) samples in Korean products. Conclusions: The use of CMIT and MIT in children's products is prohibited in Korea and the European Union (EU). The detection of CMIT in Chinese clay products suggests that management is necessary for imported products. It is necessary to review the safety and regulatory status for OIT because OIT was used as a substitute for CMIT and MIT in Korean products.

Method validation for quantitative analyzing aflatoxin productivity in Aspergillus sp. isolated from soybean paste

  • SeongEui Yoo;WooSoo Jeong;Soo-Hwan Yeo;So-Young Kim
    • Food Science and Preservation
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    • v.30 no.1
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    • pp.28-41
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    • 2023
  • Non-aflatoxigenic Aspergillus oryzae and aflatoxigenic A. flavus cannot be clearly identified by partial sequencing of the internal transcribed spacer (ITS) and 18S ribosomal ribonucleic acid (18S rRNA) regions. This study aimed to compare the accuracy among three aflatoxin detection methods using ultra-performance liquid chromatography (UPLC), high-performance liquid chromatography (HPLC), and an enzyme-linked immunosorbent assay (ELISA) kit and to select the non-aflatoxigenic Aspergillus sp. isolated from soybean paste. All analytical methods were suitable according to the international standards of Codex Alimentarius FAO-WHO (CODEX) or the Ministry of Food and Drug Safety (MFDS). UPLC exhibited the best of limit of detection (LOD) and limit of quantification (LOQ). Based on UPLC, HPLC, and the ELISA kit assay, the P5 and P7 strains isolated from soybean paste had 1,663.49, 1,468.12, and >20 ㎍/kg and 1,470.08, 1,056.73, and >20 ㎍/kg, respectively, detected and re-identified as A. flavus. In contrast, the P3 and P4 strains (A. oryzae), which were detected below the MFDS standards in all assays, were confirmed as non-aflatoxigenic fungi. Among the methods evaluated for quantitative analysis of aflatoxin, UPLC and HPLC are superior in terms of accuracy, and the ELISA kit rapidly detects low concentrations of aflatoxin. Furthermore, this study demonstrates that any Aspergillus sp. isolated for use as a fermentation starter should be analyzed for potential aflatoxin production using UPLC and HPLC for accurate quantitative analysis or ELISA for the rapid detection of low-level concentrations of aflatoxin.