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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.

A Microsporidian Parasite - $Lb_{ms}$ (Protozoa - Microspora) Infecting Lamerin Breed of the Silkworm Bombyx mori L. (Lepidoptera - Bombycidae)

  • Bhat Shabir Ahmad;Nataraju B.
    • International Journal of Industrial Entomology and Biomaterials
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    • v.12 no.1
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    • pp.41-43
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    • 2006
  • Lamerin breed of the silkworm Bombyx mori L. is the only mulberry silkworm breed which survives with an associated microsporidian $(Lb_{ms})$ infection from generations. This present comparative investigation has produced information on the influence of $Lb_{ms}$ on the growth and development of the breed. The $Lb_{ms}$ transmits tranovarially as well as perorally at low level. Larvae developed from the eggs laid by female, infected with $Lb_{ms}$ were as normal as larvae developed from the eggs laid by healthy female. In infected tissues early developmental stages and mature spores located intracellularly but did not show hypertrophy of cells of the host. The meronts and sporonts measures $0.46{\pm}0.25,\;1.11{\pm}0.05{\mu}m$ in length and $0.32{\pm}0.05,\;0.78{\pm}0.10{\mu}m$ in width respectively. The mature spore measures $4.36{\pm}0.06{\mu}m$ in length and $2.14{\pm}0.01{\mu}m$ in width.

Anthraquinone Productivity by the Cultures of Adventitious Roots and Hairy Roots from Curled Dock (Rumex crispus) (소리쟁이 (Rumex crispus)의 부정근과 모상근 배양에 의한 Anthraquinone 생산성)

  • 장석원;김인현;한태진
    • Korean Journal of Plant Tissue Culture
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    • v.26 no.1
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    • pp.7-14
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    • 1999
  • In order to survey anthraquinone productivity from in vitro root culture, transformed hairy roots of Rumex crispus were induced from leaf segments by infection with Agrobacterium rhizogenes strain $A_4$ and compared with adventitious roots. The optimum condition of adventitious root formation from leaf segments was 5 $\mu$M NAA added to MS medium. Mannopine was detected in the extract of hairy roots by paper electrophoresis, but not in adventitious roots. Secondary root tips of both adventitious roots and hairy roots elongated without lateral root branching in hormone free MS medium, but primary root tips showed more rapid growth with extensive lateral root branching. MS basal medium was the best for growth of the adventious roots and hairy roots for anthraquinone content. Adventitious root tips and hairy root tips cultured in liquid MS medium supplemented with 0.05 $\mu$M NAA and 0.1 $\mu$M kinetin (contained 5% sucrose) showed the maximal growth and anthraquinone content. Anthraquinone content of hairy roots was increased by the culture periods, but was reduced after 25 days of culture.

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Quantitative analysis of 3-MCPD in water using LC-MS (LC-MS를 이용한 수용액중의 3-MCPD 정량)

  • Park, Gyo-Beom;Kim, Yong-Hwa;Kim, Jin-Sung;Jeong, Ja-Young;Kim, Choong-Yong;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.198-203
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    • 2007
  • The analysis method of 3-Monochloropropane-1,2-diol (3-MCPD) compound in water was developed using liquid chromatography with mass spectrometric detection. Aqueous solution was controlled in strong basic condition with sodium hydroxide, and then $25{\mu}L$ of benzoyl chloride was added to the solution for the derivatization of 3-MCPD. The derivative was extracted using pentane and analyzed by the selected ion monitoring (SIM) method of LC-MS. The results of analyses showed that the calibration curves was in the range of 1.0 to $100{\mu}g/mL$ with a good linearity (correlation coefficient of $r^2=0.992$) and limit of detection was below $0.01{\mu}g/mL$. The recoveries of this analysis method by LC-MS were 92.3-98.0 %.

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
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    • v.32 no.3
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    • pp.193-198
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    • 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.

Analysis and Uncertainty Estimation of Zearalenone in Cereal-Based Products by LC-MS/MS (LC-MS/MS를 이용한 곡류가공품의 제랄레논 분석과 측정불확도 추정)

  • Choi, Eun Jung;Kang, Sung Tae;Jung, So Young;Shin, Jae Min;Jang, Min Su;Lee, Sang Me;Kim, Jung Hun;Chae, Young Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.658-665
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    • 2012
  • A survey of zearalenone contamination was conducted on cereal-based products by using an immunoaffinity column with LC-MS/MS. The calibration curve showed good lineality, with correlation coefficients ($R^2$) of 0.999 in the concentration range from 1 to 250 ng/mL. The limits of detection and quantification were approximately $0.3{\mu}g/kg$ and $1.0{\mu}g/kg$, respectively. The recoveries in the barley tea, Misutgaru and snack ranged from 73.6-107.8%. Zearalenone was detected in 10 samples (11.2% incidence). The highest zearalenone contamination level was $29.7{\mu}g/kg$ in the Misutgaru. This survey was conducted with uncertainty of measurement. The expanded uncertainty for zearalenone was estimated to be $44.9{\pm}5.0{\mu}g/kg$ (k=2, 95% confidence level) and $128.7{\pm}7.9{\mu}g/kg$ (k=2, 95% confidence level) for barley tea, $30.7{\pm}5.8{\mu}g/kg$ (k=2, 95% confidence level) and $173.7{\pm}14.9{\mu}g/kg$ (k=2.26, 95% confidence level) for Misutgaru, and $37.2{\pm}7.4{\mu}g/kg$ (k=2.31, 95% confidence level) and $151.0{\pm}10.4{\mu}g/kg$ (k=2, 95% confidence level) snack at the level of $41.7{\mu}g/kg$ and $166.7{\mu}g/kg$, respectively.

Quantitative Analysis of the Marker Constituents in Yongdamsagan-Tang using Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry (LC-ESI-MS/MS를 이용한 용담사간탕의 주요 성분 분석)

  • Seo, Chang-Seob;Ha, Hyekyung
    • Korean Journal of Pharmacognosy
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    • v.48 no.4
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    • pp.320-328
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    • 2017
  • Yongdamsagan-tang has been used to treat the urinary disorders, acute- and chronic-urethritis, and cystitis in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous analysis of the 20 bioactive marker compounds, geniposidic acid, chlorogenic acid, geniposide, liquiritin apioside, acteoside, calceolarioside B, liquiritin, nodakenin, baicalin, liquiritigenin, wogonoside, baicalein, glycyrrhizin, wogonin, glycyrrhizin, wogonin, saikosaponin A, decursin, decursinol angelate, alisol B, alisol B acetate, and pachymic acid in traditional herbal formula, Yongdamsagan-tang. Chromatographic separations of all marker compounds were conducted using a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization source in the positive and negative modes. The flow rate was 0.3 mL/min and injection volume was $2.0{\mu}L$. The correlation coefficient of 20 marker compounds in the test ranges was 0.9943-1.0000. The limits of detection and quantification values of the all marker components were 0.11-6.66 and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the optimized LC-ESI-MS/MS method, three compounds, geniposidic acid (from Plantaginis Semen), alisol B (from Alismatis Rhizoma), and pachymic acid (from Poria Sclerotium), were not detected in this sample. While the amounts of the 17 compounds except for the geniposidic acid, alisol B, and pachymic acid were $0.04-548.13{\mu}g/g$ in Yongdamsagan-tang sample. Among these compounds, baicalin, bioactive marker compound of Scutellariae Radix, was detected at the highest amount as a $548.13{\mu}g/g$.

Comparative analysis of glycerin in cosmetics by LC/MS and 1H NMR (LC/MS와 1H NMR을 이용한 화장품속의 글리세린 비교분석)

  • Park, Gyo-Beom;Park, Chan Jo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.400-405
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    • 2007
  • The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

Effect of Thidiazuron on the Formation of Micro-tubers and Plantlet Regeneration of Pinellia ternata T. (Thidiazuron이 반하(半夏)의 자구(子球) 및 식물체 재생에 미치는 영향)

  • Kim, Jae-Kwang;Cho, Hye-Kyoung;Yu, Chang-Yeon;Ahn, Sang-Deuk;Lim, Hak-Tae
    • Korean Journal of Medicinal Crop Science
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    • v.5 no.1
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    • pp.21-27
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    • 1997
  • This experiments were conducted to determine the effect of thidiazuron on forming tuberlets and plant regeneration of Pinellia ternata T. by tissue culture. The addition of $5\;{\mu}M$ TDZ to the medium had better regeneration than that of any other treatments of NAA and TDZ. At the combination treatments of NAA and TDZ, as the level of thidiazuron increased, the rate of shoot regeneration was incresed while the increment of NAA concentration inhibited the rate of shoot regeneration. The supplement of $5\;{\mu}M$ thidiazuron produced the best number of micro-tubers per explant and the number of micro-tuber formed was 25 in MS medium and 29 in MG medium on 30 day culture, respectively. Microtuber formation was the best on MG medium with 1.0 mg/l NAA and $5\;{\mu}M$ thidiazuron. MG medium was superior to MS and B5 medium for the growth of tuberlets. Half strength of MS medium with NAA 2 mg/l was the most effective for root formation. Rooting ability on nursery soil of plantlets produced in in vjtro was good as a 80% after 3 weeks.

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Analysis of Glyphosate and Glufosinate in Animal Feeds using LC-MS/MS (LC-MS/MS를 이용한 동물 사료 내 글라이포세이트 및 글루포시네이트 분석)

  • Lee, Ji-Su;Kim, Wanseo;Yang, Heedeuk;Park, Na-Youn;Jung, Woong;Kim, Junghoan;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.63 no.5
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    • pp.342-345
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    • 2019
  • The standards for the contents of glyphosate and glufosinate in foods are specific and well categorized. However, the standard of content in animal feeds is relatively inadequate and the classification is insufficient. There is also constant debate about the risk of glyphosate and glufosinate to human health, but the risk to animals has not been well studied. In this study, we established an analytical method in feeds that is estimated to be the path for animals to ingest glyphosate. The solvent extraction was carried out using 25% methanol. After centrifugation, samples were purified using solid phase extraction (SPE) and quantitatively analysed using LC-MS/MS after concentrated. Assessment of validation was conducted through detection limits, accuracy, and precision tests. The detection limits for the established method were 1.8 of ${\mu}g/kg$ of glufosinate and $2.4{\mu}g/kg$ of glyphosate. Accuracy was ranged from 94.4% to 103.4% and precision was range from 1.5% to 7.2%. Glufosinate was detected in one sample ($ND{\sim}8.8{\mu}g/kg$) and glyphosate was detected in all but one sample ($ND{\sim}337.0{\mu}g/kg$) by applying the analytical method to animal feeds (n=13).