• Title/Summary/Keyword: MS0

Search Result 4,759, Processing Time 0.034 seconds

Analysis of Carbonyl Compounds using DNPH Cartridge with LC-MS (DNPH cartridge/LC-MS 방법에 의한 카르보닐화합물 분석에 관한 연구)

  • Cho Deok-Hee;Song Il-Seok
    • Journal of Korean Society for Atmospheric Environment
    • /
    • v.22 no.2
    • /
    • pp.201-208
    • /
    • 2006
  • Several carbonyl compounds are important because of their irritant and toxic properties, mutagenicity and carcinogenicity. Therefore, they are regulated in korean odor emission standard. In this study, atmospheric pressure ionization-mass spectrometry(API-MS) is used for the analysis of carbonyl compounds after derivatization with 2, 4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation. In the negative ion mode, the $[M-H]^-$ pseudomolecular ions are most abundant for the carbonyls. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearities ($r^2$) for carbonyls were $0.9977{\sim}0.9999$ when analyte concentration ranges from $25\;to\;250{\mu}g/L$(n=6). The relative standard deviations (%RSD) for carbonyls were $0.55{\sim}3.51%$ for concentration of $100{\mu}g/L$(n=5). The minimum detection limit (MDL) was $1.88{\mu}g/L$(0.27 ppb) for i-valeraldehyde. It was shown that LC-MS method has a great potential for carbonyl compounds analysis.

A study on the pretreatment of egg and dried pork for determination of selenium using ICP/MS (ICP/MS를 이용한 계란 및 건조돼지고기 중 셀렌 분석을 위한 전처리 방법 연구)

  • Park, Kyung-Su;Kim, Sun-Tae
    • Analytical Science and Technology
    • /
    • v.14 no.6
    • /
    • pp.465-470
    • /
    • 2001
  • A pretreatment procedure was performed to improve recovery of selenium from enriched egg and dried pork. Samples were digested with only $HNO_3$ in beaker at $150^{\circ}C$ for 3 hrs, and Se was determined by ICP-MS. Recovery of selenium was 94.2%, and its C.V. value was 2.48%. The analytical results of Se by this method were 0.13 - 2.71 mg/kg for egg and 0.36 - 4.19 mg/kg for dried pork.

  • PDF

Optimal concentrations of plant growth regulators and AgNO3 for the improvement of regeneration efficiency in Chrysanthemum morifolium 'Ohblang' (국화 '오블랑'의 재생 효율 증진을 위한 식물생장조절제와 AgNO3 적정 농도 선별)

  • Yeo Jin Youn;Yong Joon Yang
    • Journal of Plant Biotechnology
    • /
    • v.50
    • /
    • pp.169-175
    • /
    • 2023
  • A plant regeneration system was developed through shoot organogenesis from in vitro leaf explants of Chrysanthemum morifolium 'Ohblang'. The effects of different concentrations of plant growth regulators and AgNO3 on efficient shoot regeneration and inhibition of browning were evaluated in chrysanthemum. The explants were cultured on MS shoot induction medium supplemented with 12 combination treatments of 6-benzyladenine (BA) 0.5, 1.0 and 2.0 mg/L, and α-naphthaleneacetic acid (NAA) 0.2, 0.5, 1.0 and 2.0 mg/L in darkness for 6 weeks and cultured under a 16/8 h photoperiod for 6 weeks. The highest shoot regeneration was obtained from the explants cultured on the medium with 1.0 mg/L BA and 1.0 mg/L NAA. Based on this result, AgNO3 was added to a shoot induction medium containing MS salts, vitamins, 1.0 mg/L BA, 1.0 mg/L NAA, 30 g/L sucrose, and 6 g/L agar to reduce browning of chrysanthemum leaf explants. In the control treatment without AgNO3, leaf explants turned brown at the cut edge; however, browning was not observed in AgNO3 treatments. Shoot organogenesis was higher at low concentrations of AgNO3 and decreased with an increase in AgNO3 concentration. The explants cultured on shoot induction medium (MS salts, vitamins, 1.0 mg/L BA, 1.0 mg/L NAA) with 1 mg/L of AgNO3 produced the highest shoot regeneration with 2.6 shoots per explants and a browning index of 0.7. When the regenerated shoots were detached from the explants and cultured on MS medium, the shoots were elongated and rooted successfully.

Determination of Amitrole in Water Samples by Evaporation and GC/MS (증발법과 GC/MS를 이용한 수질 시료 중의 Amitrole의 분석법 연구)

  • Yoon, So Hee;Hong, Ji Eun;Pyo, Hee Soo;Park, Song Ja
    • Analytical Science and Technology
    • /
    • v.16 no.6
    • /
    • pp.483-487
    • /
    • 2003
  • Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.

Determination of the Impurities in Isoprene by GC/MS (GC/MS를 이용한 이소프렌 중 불순물 분석)

  • Lee, Hyunjoo;Ahn, Byoung Sung;Suh, InSuk;Kwon, Young Soo
    • Analytical Science and Technology
    • /
    • v.14 no.4
    • /
    • pp.300-305
    • /
    • 2001
  • The impurities in isoprene were determined using GC/MS. There were good linearities (above $R^2=0.996$) in the range of the $1.0-50{\mu}g/mL$ and 0.5-5.0%, and the detection limits of the method were below $0.1{\mu}g/mL$ for each impurities. Reagent-grade isoprene contained isopropenyl acetylene and 2-butyne at $10-50{\mu}g/mL$ and the concentrations of cis-piperylene, trans-piperylene, cyclopentadiene and dicyclopentadiene were below $1{\mu}g/mL$. The analysis confirmed that the reagent grade isoprene could be obtained from the distillation of C5 fractions.

  • PDF

Association of Plasma Osteoprotegerin with Adiponectin and Difference according to Obesity in Men with Metabolic Syndrome (대사증후군 남성에서의 혈중 Osteoprotegerin의 아디포넥틴과의 상관성과 비만도에 따른 차이)

  • Na, Woo-Ri;Sohn, Cheong-Min
    • Korean Journal of Community Nutrition
    • /
    • v.16 no.6
    • /
    • pp.762-770
    • /
    • 2011
  • Osteoprotegerin (OPG) plays a core role in bone reformation by antagonizing the effect of receptor activator of nuclear factor ${\kappa}$-B ligand (RANKL), and mediates vascular calcification in cardiovascular disease patients. Thus, we aimed to examine the relationship between serum OPG levels and cardiovascular factors and inflammatory markers in metabolic syndrome patients (MS). This cross-sectional study included 96 men who visited the diet clinic between May and July 2011. Patients were classified into 2 groups based on NCEP-ATP guidelines: normal and with MS (n = 50 and 46, respectively). Physical measurements, biochemical assay were measured. Serum OPG and IL-6, diponectin and hs-CRP were assessed. MS were aged $50.02{\pm}10.85$ years, and normal patients $52.07{\pm}9.56$ years, with no significant differences. Significant differences were not observed in BMI between the 2 groups. Moreover, significant differences were not observed in serum OPG, however, the serum OPG level ($4.41{\pm}1.86pmol/L$) differed significantly between an overweight MS (BMI > 25) and normal patients. OPG was correlated to age (r = 0.410, p = 0.000), HDL-cholesterol (r = 0.209, p = 0.015), and log adiponectin (r = 0.175, p = 0.042). Multiple regression analyses using the enter method showed that age (${\beta}$ = 0.412, p = 0.000) and BMI (${\beta}$ = 0.265, p = 0.000) considerably affected OPG. In conclusion, out study showed that serum OPG levels are correlated with cardiovascular risk factors, such as BMI, HDL-cholesterol and adiponectin in MS and adiponectin, suggesting that serum OPG has potential as a cardiovascular disease indicator and predictor.

Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
    • /
    • v.53 no.1
    • /
    • pp.25-30
    • /
    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

Development of Analytical Method for Determination of Baicalin, Eleutheroside E, and Ligustilide by LC-MS/MS in Raw Materials of Health Functional Foods (LC-MS/MS를 이용한 건강기능식품 원료 중 바이칼린, 엘레우테로사이드 E, 리구스틸라이드 동시분석법 개발)

  • Keum, Eun Hee;Chung, So Young;Lee, Jin Hee;Kim, Meehye
    • Journal of Food Hygiene and Safety
    • /
    • v.32 no.3
    • /
    • pp.193-198
    • /
    • 2017
  • Scutellaria baicalensis, Eleutherococcus senticosus, and Angelica sinensis have been used as raw materials for health functional foods. This study was conducted to develop a novel method to analyze levels of baicalin (Scutellaria baicalensis), eleutheroside E (Eleutherococcus senticosus), and ligustilide (Angelica sinensis) simultaneously in health functional foods. The methanol extracted samples were analyzed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode and the negative ion mode using multiple reaction monitoring. Standard calibration curves confirmed linearity with the correlation coefficient ($r^2$) of > 0.99 at $100-2000{\mu}g/mL$ concentration range. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $13.0{\sim}35.2{\mu}g/L$ and $39.3{\sim}106.7{\mu}g/L$, respectively. The recovery results ranged between 91.4~109.9% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high accuracy and acceptable precision. The new method would be an effective tool to analyze baicalin, eleutheroside E, and ligustilide simultaneously in raw materials of health functional foods.

Development of Enhanced Analytical Method for Perchlorate in Food by IC-MS/MS with an Internal Standard (IC-MS/MS와 내부표준물질을 이용한 식품 중 perchlorate 분석법 개선)

  • Yang, Min-June;Kim, Jong-Sung;Han, Jong-Hun;Her, Nam-Guk
    • Korean Journal of Food Science and Technology
    • /
    • v.43 no.5
    • /
    • pp.532-536
    • /
    • 2011
  • The internal standard method using ion chromatography combined with tandem mass spectrometry (IC-MS/MS) for quantifying perchlorate in different types of food was established. Because the presence of ions and other biomolecules in matrices usually interrupts accurate determination of perchlorate, it is necessary to develop efficient, reproducible method to determine perchlorate concentrations in food. In this study, the internal standard method was compared with the external standard method to determine perchlorate concentrations in standard samples. The obtained method detection limit (MDL) for perchlorate was 0.005 ${\mu}g/L$ for bottled water, 0.12 ${\mu}g/L$ for milk, 0.27 ${\mu}g/kg$ for rice, 0.16 ${\mu}g/kg$ for vegetables, and 0.07 ${\mu}g/kg$ for seaweed, respectively. The limit of quantitation (LOQ) was calculated by multiplying the MDL by 7. The recoveries of perchlorate from food samples spiked with perchlorate ranged from 98 to 105% and their percent relative standard deviation (%RSD) levels were <20%. This method was successfully applied for the quantitative determination of perchlorate in various kinds of food.

Survey and method validation of simultaneous quantitative analysis of T-2 and HT-2 toxins in cereals (곡류 중 T-2 및 HT-2 독소 동시 정량분석의 유효성 검증 및 실태조사)

  • Paek, Ockjin;Kang, Teabeom
    • Food Science and Preservation
    • /
    • v.22 no.4
    • /
    • pp.559-566
    • /
    • 2015
  • The aim of this study was to develop an analytical method for determination of T-2 toxin and HT-2 toxin level in cereals and to survey their levels using LC-MS/MS. The T-2 and HT-2 toxins were simultaneously analyzed by electrospray ionization with a positive ion mode and multiple reaction monitoring (MRM) after filteration and immuno-affinity column clean-up. A matrix-matched standard calibration used for quantification and recoveries of T-2 and HT-3 toxins were in the range of $100.6{\pm}7.2%$ and $96.8{\pm}9.4%$, respectively. Limits of detection and quantification of T-2 and HT-2 toxins were estimated to be 0.5 and $1.5{\mu}g/kg$, respectively. Each repeatability (RSRr) of T-2 and HT-2 toxins was determined to be 0.9~6.0%, and 4.9~6.1%, respectively. Total 115 samples cereals were collected from 9 types of cereals for analysis. The positive percentages of T-2 and HT-2 toxins obtained from collected samples were found to be 72% and 80%, respectively. The contamination level of T-2 toxin and HT-2 toxin in cereals were $37.1{\mu}g/kg$, and $5.4{\mu}g/kg$, respectively. Therefore, this study suggests that the developed method could be an useful analytical method to determine the T-2 and HT-2 toxin level in cereals and the present data could be used as a reference to estimate the risk assessment.