• Title/Summary/Keyword: LC20

Search Result 644, Processing Time 0.026 seconds

Monitoring of Malachite Green in Freshwater Fish using LC-MS/MS (LC-MS/MS를 이용한 담수 어류 중 말라카이트 그린 분석)

  • Choi, Hee-jin;Yuk, Dong-Hyun;Park, Young-Ae;Jung, Bo-Kyeng;Hong, Mi-Sun;Yoon, Yong-Tae;Yi, Hye-Jin;Kim, Youn-Cheon;Park, Sung-Kyu;Kim, Moo-Sang;Jung, Kweon
    • Journal of Food Hygiene and Safety
    • /
    • v.31 no.1
    • /
    • pp.15-20
    • /
    • 2016
  • Malachite green was measured in 200 freshwater fish collected from local markets in Seoul using HPLC-DAD and LC-MS/MS. LC-MS/MS method was validated by linearity, accuracy, precision and limits of detection and quantification according to the CODEX's recommendation and HPLC-DAD method was applied according to the Food Code. Malachite green levels above the quantification limit of the LC-MS/MS were determined 18.5% (37) but just 1 fish was shown to contain malachite green by HPLC-DAD. Of 83 domestic fish, 21 fish were detected malachite green (25.3%). Of 117 fish from China, just 16 fish were detected malachite green (13.4%). In detection rate by species carp (35.0%), Crucian carp (30.4%), cat fish (28.0%), Korean bull head (23.8%), snake head (20.0%), eel (10.5%) and loach (7.8%) were in order. Especially, fish collected at summer were shown to contain malachite green frequently; the detection rate was 54.8%.

A New Analytical Method for Erythromycin in Fish by Liquid Chromatography/Tandem Mass Spectrometry

  • Park, Mi-Jung;Park, Mi-Seon;Lee, Tae-Seek;Shin, Il-Shik
    • Food Science and Biotechnology
    • /
    • v.17 no.3
    • /
    • pp.508-513
    • /
    • 2008
  • Erythromycin has been used to treat Streptococosis, Edwardsiel1osis, Vibriosis, Bacterial enteritis in the cultured fish. In this study, a rapid and effective erythromycin analysis method with new sample treatment protocol and liquid chromatography/tandem mass spectrometry (LC/MS/MS) system for fish products was developed. For the erythromycin extraction from fish muscle, the solvent mixture composed of 0.2% meta-phosphoric acid and methanol (6:4) showed good recovery rate, and the optimum extraction solvent volume was 20 mL. Erythromycin detection using LC/MS/MS were carried out under electro spray ionization (ESI) positive condition and erythromycin mass value 576.2 and 157.9. And the detection limit of the established method was 0.005 mg/kg in fish products. The recovery rate of the developed method applied to the fish species were as following, olive flounder, $87.6{\pm}5.0%$; black rockfish, $87.2{\pm}6.4%$; eel, $85.2{\pm}4.8%$; and rainbow trout, $86.0{\pm}6.2%$. In the established method in this study, the correlation of coefficient values ($R^2$) of erythromycin calibration curve (n=11) was 0.9998.

Optimization of Enzyme Digestion Conditions for Quantification of Glycated Hemoglobin Using Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry

  • Jeong, Ji-Seon
    • Mass Spectrometry Letters
    • /
    • v.5 no.2
    • /
    • pp.52-56
    • /
    • 2014
  • Glycated hemoglobin (HbA1c) is used as an index of mean glycemia over prolonged periods. This study describes an optimization of enzyme digestion conditions for quantification of non-glycated hemoglobin (HbA0) and HbA1c as diagnostic markers of diabetes mellitus. Both HbA0 and HbA1c were quantitatively determined followed by enzyme digestion using isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) with synthesized N-terminal hexapeptides as standards and synthesized isotope labeled hexapeptides as internal standards. Prior to quantification, each peptide was additionally quantified by amino acid composition analysis using ID-LC-MS/MS via acid hydrolysis. Each parameter was considered strictly as a means to improve digestion efficiency and repeatability. Digestion of hemoglobin was optimized when using 100 mM ammonium acetate (pH 4.2) and a Glu-C-to-HbA1c ratio of 1:50 at $37^{\circ}C$ for 20 h. Quantification was satisfactorily reproducible with a 2.6% relative standard deviation. These conditions were recommended for a primary reference method of HbA1c quantification and for the certification of HbA1c reference material.

Investigation of Domoic acid in Shellfish Collected from Korean Fish Retail Outlets

  • Choi, Kyu-Duck;Lee, Jong-Soo;Lee, Jong-Ok;Oh, Keum-Soon;Shin, Il-Shik
    • Food Science and Biotechnology
    • /
    • v.18 no.4
    • /
    • pp.842-848
    • /
    • 2009
  • The purpose of this study was to determine the extent of domoic acid (DA) a potent neurotoxin, responsible for the syndrome amnesic shellfish poisoning (ASP) contamination of various species of bivalve shellfish purchased from fish market in Korea and the implications for food safety. Liquid chromatography (LC) methods were applied to quantify DA in shellfish after sample clean-up using solid-phase extraction (SPE) with strong anion exchange (SAX) cartridges. Toxin detection was achieved using photodiode array ultraviolet (LC-UV) and electrospray ionization-mass (LC-ESI-MS). DA was identified in 4 bivalve shellfishes of 872 shellfishes collected from March, 2006 to October, 2007 in Korea. DA amount of 3 surf clams (Mactra veneriformis) collected at Seoul, Daejeon, and Daegu were 4.13, 1.99, and 1.94 mg/kg, respectively. DA amount of 1 pink butterfly shell (Peronidia venulosa) collected at Seoul was 3.02 mg DA/kg. The amounts of DA that were present in 4 bivalve shellfishes were within EU guideline limits for sale of shellfish (20 mg DA/kg).

Bioassays On marine Organisms: Acute Toxicity Test Of mercury, Cadmium And Copper To Arkshell, Anadara broughtonii, From Jin-Dong Bay, And To Oyster, Crassostrea gigas, From Kwang-Do Bay, South Coast Of Korea

  • Park, Joo-Suck;Kim, Hak-Gyoon
    • 한국해양학회지
    • /
    • v.13 no.1
    • /
    • pp.35-43
    • /
    • 1978
  • Short-term acute toxicity of mercury, cadmium and copper to arkshell, Anadara broughtonii, and to oyster, Crassostrea gigas, was determinedby static bioassays from 20 May to 27 June in 1977. During the observations of the opening rate of the shell mercury was the most sensitive toxicant of the three toxic substances to the test animals and caused them to close their shellvalves together after being exposed to a mercury solution for an hour during the test. Opening rate to cadmium and copper increased gradually at the higher concentration. the 96hr-LC50 values for the test animals are 4.84mg/l for mercury and 1.86mg/l for cadmium, while the 72hr-LC50 value for copper is 0.31mg/l. the death rate of oysters for cadmium showed lower than that of the mercury and copper test solutions. The 96hr-LC50 values of mercury, copper and cadmium were 1.1mg/l, 2.54mg/l and 19.5mg/l, respectively. For oysters mercury was the most toxic substance, and cadmium was the least toxic one. the medium lethal time (LT 50) value decreased gradually at higher concentration of heavy metals. The LT 50 of 2mg/l was found within 96 hours ofr copper, 104 hours for mercury and 121 hours for cadmium. The lethal threshold concentrations for 7 days were found to be about 1mg/l for mercury and copper, and 2mg/l for cadmium.

  • PDF

Study on the Fringe Field Switching (FFS) Mode with the Positive Dielectric Anisotropy for the Fast Response Time (유전율 이방성이 양인 액정을 이용한 고속응답용 FFS 모드)

  • 김미숙;김향율;송성훈;양석만;이성규;임영진;이승희
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
    • /
    • v.17 no.7
    • /
    • pp.754-759
    • /
    • 2004
  • We have studied the fringe field switching (FFS) mode with the positive dielectric anisotropy for the fast response time. The factors such as the physical properties of the LC, the cell gap, and the rubbing angle were critical for the fast response time of the FFS mode. The response time became 10 ms faster when the rotational viscosity of the new LC is 20 mPa.s lower than the conventional LC. When the cell gap changed from 3.6 ${\mu}{\textrm}{m}$ to 3.0 ${\mu}{\textrm}{m}$, it was possible to achieve the total response time and response times associated with grey-to-grey transitions under 16 ms. And the response times including grey-to-grey transitions become fast as the rubbing angle decreases.

Identification of Antioxidative Constituents from Polygonum aviculare using LC-MS Coupled with DPPH Assay

  • Shin, Hyeji;Chung, Hayeon;Park, Byoungduck;Lee, Ki Yong
    • Natural Product Sciences
    • /
    • v.22 no.1
    • /
    • pp.64-69
    • /
    • 2016
  • A method for simultaneously identifying antioxidative compounds was developed using time-based LC-MS coupled with DPPH assay regardless of the time consuming process. The methanolic extract of Polygonum aviculare (Polygonaceae) showed significant DPPH radical scavenging activity. Time-based DPPH assay for simultaneous identification of active compounds from the extracts of P. aviculare was used. Major peaks of ethyl acetate fraction of P. aviculare showed high DPPH radical scavenging activity. A simple phenolic compound (1) and six flavonoids (2-7) were isolated from the ethyl acetate fraction of P. aviculare by silica gel and sephadex LH-20 column chromatography. The structures of seven compounds were determined to be protocatechuic acid (1), catechin (2), myricitrin (3), epicatechin-3-O-gallate (4), avicularin (5), quercitrin (6), and juglanin (7) based on the analysis of the $^1H$-NMR, $^{13}C$-NMR and ESI-MS data. All compounds exhibited significant antioxidant activity on DPPH assay and active compounds were well correlated with predicted one.

Changes in Milk Production and Metabolic Parameters by Feeding Lactating Cows Based on Different Ratios of Corn Silage: Alfalfa Hay with Addition of Extruded Soybeans

  • Yana, Rong;Zhang, Ruizhong;Zhang, Xian;Jiang, Chao;Han, Jian-Guo;Zhang, Ying-Jun
    • Asian-Australasian Journal of Animal Sciences
    • /
    • v.24 no.6
    • /
    • pp.800-809
    • /
    • 2011
  • The objective of this study was to investigate the effects of different ratios of corn silage (CS): alfalfa hay (AH), and extruded soybeans (ESB) on milk yield, milk composition, blood metabolites, and fatty acids in milk fat and plasma. Ninety multiparous Holstein cows were arranged in a randomized block design experiment which lasted 14 weeks. Treatments were arranged as a $3{\times}3$ factorial with 0%, 5% or 10% ESB (dry matter basis) and three forage treatments: I) 30% CS, 10% AH and 10% Leymus chinense hay (LC); ii) 20% corn silage, 20% alfalfa hay and 10% LC; iii) 10% CS, 30% AH and 10% LC. Cows were allowed to consume a total mixed ration ad libitum. There was no change of dry matter intake when cows were fed the experimental diets. As more AH was added to the diets, milk yield, milk protein content and yield, and trans9, cis11-conjugated linoleic acids (CLA) concentrations in milk fat and plasma increased. When ESB were supplemented to the diets, milk yield, and trans9, cis11-CLA concentration in milk fat and plasma increased. When 10% ESB was added to the diet containing 30% AH the trans9, cis11-CLA content (1.46 g/100 g of total fatty acids) in milk was the highest among all treatments. These results suggests that AH could replace part of a CS diet and be a good forage source of diet for dairy cows to improve milk yield and milk composition. Meanwhile, ESB could be included in the diet with high AH to improve production performance of dairy cows.

Keratanase II Digestion Accompanied with a Liquid Chromatography/Tandem Mass Spectrometry for Urinary Keratan Sulfate Quantitative Analysis

  • Chuang, Chih-Kuang;Lin, Hsiang-Yu;Wang, Tuen-Jen;Huang, Sung-Fa;Lin, Shuan-Pei
    • Journal of mucopolysaccharidosis and rare diseases
    • /
    • v.3 no.1
    • /
    • pp.20-27
    • /
    • 2017
  • Purpose: Mucopolysaccharidosis IV (MPS IV) is a disease characterized by deficient activity of N-acetylgalactosamine-6-sulfatase (GALNS) causing excessive lysosomal storage of keratan sulfate (KS). The identification of the relevant disaccharide units of KS after keratanase II digestion followed by liquid chromatography/tandem mass spectrometry detection (LC-MS/MS) is validated and applicable for the preliminary diagnosis of MPS IV. Methods: A total of 67 urine samples were collected and analyzed from 11 MPS IV patients comprising 10 MPS IVA and one MPS IVB patients, and 56 normal controls. Urinary glycosaminoglycan was first precipitated by the Alcian blue method followed by a digestion of keratanase II. The protonated species of the digested disaccharide products were detected by using multiple reaction monitoring experiment. Results: One particular disaccharide of KS was selected. The transition mass-to-charge (m/z) of the parent ion and its daughter ion after collision was $462.0{\rightarrow}97.0$, whereas the chondrosine used as an internal standard in this assay was m/z $353.9{\rightarrow}73.0$. The results corresponded well with the two-dimensional electrophoresis method. The quantities of urinary KS were significantly raised in confirmed MPS IV patients when comparing with those of normal controls ($170.2{\pm}81.1$ vs. $4.06{\pm}1.92{\mu}g/mL$). Conclusion: The LC-MS/MS method for MPS IVA determination is specific, sensitive, validated, and applicable for urinary KS quantification. This method can be used not only as a first-line biochemistry examination of MPS IVA, but also as an outcome survey after enzyme replacement therapy.

Effects of Alkoxy Side Chain on the Properties of Wholly Aromatic Liquid Crystalline Polyesters with Biphenylene Units (알콕시 곁사슬기가 비페닐렌구조를 갖는 전방향족 액정폴리에스터의 물성에 미치는 영향)

  • Lee, Eung-Jae;Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
    • /
    • v.11 no.10
    • /
    • pp.4041-4046
    • /
    • 2010
  • Wholly aromatic polyesters having flexible alkoxy side chain were synthesized by direct polycondensation. The synthetic polymers have been characterized by $^1H$-NMR, FT-IR. DSC, TGA, optical polarizing microscope and X-ray diffractometer. The inherent viscosities (${\eta}_{inh}$) measured in 1,1,2,2-tetrachloroethane (TCE) were 0.46~2.41 dL/g. The polymers having side chain showed double melting transition, ie, solid-sanidic liquid crystalline (LC) phase transition ($T_{m1}$) and sanidic LC phase-nematic LC phase transition ($T_{m2}$). As incresing length of alkoxy side chain, phase transition temperatures decreased and solubilities in organic solvents incresed. The peaks of $2{\theta}\;{\simeq}5$ and $2{\theta}\;{\simeq}20$ in X-ray diffractograms are due to crystallization of polymer main chain and of long side chain, respectively.