• Title/Summary/Keyword: HPLC/UPLC

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Antimicrobial Compounds Profile During Cheonggukjang Fermentation Against Xanthomonas oryzae pv. oryzae (Xoo)

  • Son, Gun-Hee;Kim, Ji-Young;Muthaiya, Maria John;Lee, Sa-Rah;Kim, Hyang-Yeon;Lee, Choong-Hwan
    • Journal of Microbiology and Biotechnology
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    • v.21 no.11
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    • pp.1147-1150
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    • 2011
  • Xanthomonas oryzae causes rice bacterial blight, which has been reported as one of the most destructive diseases of rice. Metabolites were identified through cheonggukjang, a traditional Korean fermented soybean product fermented by the Bacillus spp., to control the bacteria. HPLC, MS, and UPLC-Q-TOF-MS analyses were performed to identify metabolites responsible for antimicrobial activity. In this analysis, the m/z values of 253.0498, 283.0600, 269.0455, 992.6287, and 1,006.6436 were identified as daidzein, glycitein, genistein, surfactin B, and surfactin A, respectively. The levels of surfactin B and surfactin A were found to be high at 24 h (4.35 ${\mu}g$/ml) and 36 h (3.43 ${\mu}g$/ml) of fermentation, respectively.

Fast and Accurate Determination of Algal Toxins in Water using Online Preconcentration and UPLC-Orbitrap Mass Spectrometry (온라인 시료주입과 UPLC-Orbitrap 질량분석법을 이용한 수질 조류독소의 고속분석방법 개발 및 환경시료적용)

  • Jang, Je-Heon;Kim, Yun-Seok;Choi, Jae-Won
    • Journal of Korean Society on Water Environment
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    • v.28 no.6
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    • pp.843-850
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    • 2012
  • Due to the fast response to algae bloom issue in drinking water treatment plant, very fast determination methodology for algal toxin is required. In this study, column switching technique based online preconcentration method was combined with high resolution full scan mass spectrometer to save sample preparation time and to obtain fast and accurate result. After parameter optimization of online preconcentration, 1mL filtered sample was directly injected to trap column with switching valve system. Next, target toxins are eluted by 98% acetonitrile and analysed with 150 - 1,100 amu scan range at 50,000 resolving power. Method detection limit (MDL) for microcystin-LR, the most toxic isomer, was 0.1 ng/mL and others such as microcystin-YR, microcystin-RR and nodularin were 0.08, 0.03 and 0.04 ng/mL, respectively. This is the best improved sensitivities with 1mL volume in the literature. Furthermore, due to the use of ultra pressure HPLC (UPLC), the whole method run was completed in 4 min. Real sample applications for 173 sample including 55 surface water and 118 treatment plant samples for raw and treated water could be done within 16 hours. In our calculation, this methodology is roughly 80% faster than the previous manual solid-phase extraction with LC-MS/MS method.

Simultaneous Determination of 8 Preservatives (6 Parabens, 2-Phenoxyethanol, and Chlorphenesin) in Cosmetics by $UPLC^{TM}$ ($UPLC^{TM}$를 이용한 화장품 중 보존제 8종(파라벤 6종, 페녹시에탄올, 클로페네신)의 동시분석)

  • Park, Jeong-Eun;Lee, So-Mi;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.33 no.4
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    • pp.263-267
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    • 2007
  • Parabens are used in nearly all types of cosmetics and toiletries because they are formulated well and have broad spectrum of activity, interness, low costs and excellent chemical stability in relation to pH. 2-phenoxyethanol and chlorphenesin are common preservatives which are usually used in combination with parabens in cosmetics. Toxicity of parabens is generally low but application of parabens to damaged or broken skin has resulted in sensitization. Moreover, the possibility of their estrogenic potential, anesthetic effects and reproductive toxicity has been reported. Consequently there are some regulations in use of parabens. And the maximum permitted concentrations of chlorphenesin and 2-phenoxyethanol in cosmetic products are authorized by the same reasons. So it is important to control and estimate the amount of parabens in products. In this article, we proposed a valid method for the simultaneous determination of 8 preservatives including parabens in a short time using ultra performance liquid $chromatography^{TM}\;(UPLC^{TM})$. Separation of eight components was achieved in less than 10 min and resolutions were reasonable (USP resolution ${\geqq}\;2$). And limit of detection and quantification were evaluated. The method was suitably validated for specificity, linearity, precision (repeatability, intermediate precision) and accuracy for assay (recovery) based on International conference on harmonisation (ICH) guideline. The method was applicable to analysis of preservatives in cosmetic products.

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.

Sample Preparation and Stability of Human Serum and Urine Based on HPLC-DAD for Metabonomics Studies

  • Liu, Yun;Sun, Xiaoming;Di, Duolong;Feng, Yuxiang;Jin, Fengling
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2156-2162
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    • 2012
  • Many literatures focus on the biological relevance and the identification of biomarkers for disease activity assessment while less attention has been paid to the development of standard procedures for sample preparation and storage based on liquid chromatography technique. The influencing factors including protein precipitation, storage temperature, storage time, and reconstitution by ultra pure water were analyzed employing HPLC-DAD. The effects were investigated from five participants over three months by principal components analysis (PCA) and the values of percent changes (PC). The samples with protein precipitation might slow the rate of bacterial enzymatic conversion. After protein precipitation, the average PC of urine samples ($0.136{\pm}0.013$, n = 5) is relatively less than that of the serum samples ($0.173{\pm}0.026$, n = 5) for three months. Minimal effects on metabolic profiles of serum and urine (PC < 0.15) are reasonable for metabolomic studies after protein precipitation and storage at $-20^{\circ}C$ for two months.

Variation of Selected Phenotypic Characteristics, Anthocyanins and Bitter Sesquiterpene Lactones in Lettuce (Lactuca sativa L.) Germplasm (상추(Lactuca sativa L.)유전자원의 형태 특성 및 Anthocyanins과 Bitter Sesquiterpene Lactones 변이)

  • Choi, Susanna;Assefa, Awraris Derbie;Lee, Jae-Eun;Hur, On-Sook;Ro, Na-Young;Lee, Ho-Sun;Noh, Jae-Jong;Hwang, Ae-Jin;Kim, Yeong-Jee;Kim, Bich-Saem;Ko, Ho-Cheol;Rhee, Ju-Hee
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2019.10a
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    • pp.95-95
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    • 2019
  • 상추(Lactuca sativa L.)는 대표적인 쌈 및 샐러드 채소로 우리나라 기준(2016년) 3,387 ha의 면적에서 86,128톤을 생산하여 엽채류 중 배추, 양배추 다음으로 많이 생산되는 작물이다. 안토시아닌(Anthocyanins)은 열매, 꽃, 줄기, 잎 등 식물계에 널리 분포되어 있는 페놀 화합물 중 하나로 적색, 자색 등의 색을 나타내는 수용성 flavonoid계 색소이다. BSLs (Bitter sesquiterpene lactones)는 항암, 항균, 해열과 염증완화에 효과가 있는 것으로 알려져 있다. 본 연구는 농촌진흥청 농업유전자원센터에서 보유 중인 상추 66자원의 형태학적 특성 및 액체크로마토그래피(HPLC, UPLC)를 이용한 안토시아닌과 BSLs성분을 분석하여 함량이 높은 자원을 선발하고자 한다. 상추시료 0.05 g을 $MeOH/H_2O/AcAc$로 추출 한 후, UPLC를 사용하여 안토시아닌 함량을 분석하였으며, 상추시료 0.25 g을 100% MeOH로 추출 한 후 HPLC를 사용하여 BSLs 함량을 분석하였다. 연구 결과, 상추 유전자원의 안토시아닌 함량 범위는 0 mg/100 g에서 371.94 mg/100 g이고, BSLs성분 함량 범위는 $60.28{\mu}g/g\;DW$에서 $2821.92{\mu}g/g\;DW$ 이었다. 상추 66자원 중 안토시아닌함량이 200 mg/100 g이상인 자원은 IT217012, IT218395, IT231524, IT231525, IT260852이며, BSLs 함량이 $1700{\mu}g/g\;DW$이상인 자원은 IT231524, IT231525, IT231527, IT264971, IT271118이다. 두 성분의 함량이 모두 높은 자원 IT231524와 IT231525 이었다. 이 두자원의 형태적 특성은 초형이 잎상추로 잎이 넓은 타원형에 가장자리 결각이 강한 자주색이다. 따라서 본 연구는 다양한 상추 유전자원의 형태학적 특성 및 BSLs, 안토시아닌 성분이 높은 자원을 선발하여 육종소재로 활용하고자 한다.

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A survey on pesticide residues of imported fruits circulated in Gyeonggido (경기도내 유통 수입과실류의 잔류농약 실태조사)

  • Cho, Yun-Sik;Kang, Jeong-Bok;Kim, Yang-Hee;Jeong, Jin-A;Huh, Jeong-Weon;Lee, So-Hyun;Lim, Young-Sik;Bae, Ho-Jeong;Kang, Heung-Gyu;Lee, Jeong-Hee;Jung, Eun-Sook;Lee, Byoung-Hoon;Park, Yong-Bok;Lee, Jong-Bok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.195-201
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    • 2012
  • We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

Identification of process generating formaldehyde in a furniture manufacturer (특정 가구 제조 공장의 포름알데히드 발생 공정 노출 평가)

  • Yoo, Kye-Mook;Lee, Mi-Young
    • Analytical Science and Technology
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    • v.27 no.5
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    • pp.243-247
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    • 2014
  • Formaldehyde is defined as carcinogen causing leukaemia, lymphoma or nasopharyngeal carcinoma at high level of exposure. Furniture-manufacturing workers can be exposed to formaldehyde, which implies serious impact on health of the workers. The authors carried out ambient monitoring of formaldehyde in the field, and identified the source of formaldehyde generated during the working process by testing the condition in the laboratory settings. After sampling formaldehyde in the air with 2,4-DNPH (2,4-dinitrophenylhydrazine) coated silica gel, we extracted formaldehyde derivative with acetonitrile and analyzed the extract using HPLC with UV detector at 360 nm. Formaldehyde was separated by ACQUITY UPLC BEH $C_{18}$ column at a flow rate of 0.5 mL/min using 45% acetonitrile as mobile phase. The workers were exposed to higher level of formaldehyde than normal air. Formaldehyde up to 0.31 ppm was detected in the process of veneer attachment, which exceeded 0.3 ppm, the ceiling value of ACGIH standard. The laboratory test of measuring formaldehyde generated from the glue and veneer used in the attachment process resulted in more formaldehyde generation as the temperature increased, and more from the veneer. Heating the veneer to $100-150^{\circ}C$ following the real condition of the manufacturing site generated 1.14-2.70 ppm of formaldehyde from the sample, which was 2-5 times higher level than Korean limit of exposure (0.5 ppm). As the workers handling and processing the veneer which was produced by wet process had high possibility to be exposed to formaldehyde, urgent improvement and management of working environment of furniture manufacturer is demanded.

A Study on the Safety of Residual Pesticides in Cereal Grains and Pulses Agricultural Products Excluding Rice (잡곡 농산물의 잔류농약 안전성 조사)

  • Han, Na-Eun;Kim, Jae-Gwan;Yun, Hee-Jeong;Kang, Min-Seong;Cho, Young-Seon;Song, Ji-Won;Kim, Byeong-Tae;Lee, Seong-Nam;Choi, Ok-Kyung
    • Journal of Food Hygiene and Safety
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    • v.37 no.1
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    • pp.1-8
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    • 2022
  • In this study, the pesticide residues in 106 commercial cereal grains were monitored from February to July 2021. For the investigation, 40 domestic and 66 imported products from large, small-to-medium sized offline and online distribution channels, were collected and analyzed by using the multiresidue method for 341 pesticides on GC/ECD, GC/NPD, GC/MSMS, UPLC/PDA, HPLC/FLD, LC/MSMS. Pesticides were detected in total of 8 samples (7.5%), of which one was from big box retailers, two from small and medium-sized distribution stores, and five from online shopping mall. Five (4.7%) samples were found to have pesticide residues greater than the maximum residue limits (MRLs). The detected pesticides in kidney beans (1 case), mung beans (6 cases), and sorghum (1 case), were MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, and pirimiphos-methyl. Specifically, an excessive amount of thiamethoxam was found from the imported mung bean (5 cases).

Modified QuEChERS Multi-Residue Analysis Method for 61 pesticides in Fruits using with HPLC and GC-ECD/NPD (HPLC 및 GC-ECD/NPD를 이용한 과일 중 61종 농약의 QuEChERS 전처리 다성분 분석법 개발)

  • Lee, Ju-Young;Hong, Su-Myeong;Kim, Taek-Kyum;Min, Zaw Win;Kim, Yang-Hyeon;Song, Kyung-Ae;Kwon, Hye-Yong;Lee, Hee-Dong;Im, Geon-Jae;Kim, Doo-Ho;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.242-256
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    • 2012
  • QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.