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Determination of Phthalate Metabolites in Korean Children's Urine by High Performance Liquid Chromatography with Triple Quadrupole Tandem Mass Spectrometry (LC/MS/MS를 이용한 어린이 소변 중 프탈레이트 대사산물 분석)

  • Kho, Young-Lim;Jeong, Jee-Yeon;Choi, Kyung-Ho;Kim, Pan-Gyi
    • Journal of Environmental Health Sciences
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    • v.34 no.4
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    • pp.271-278
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    • 2008
  • Dialkylated phthalates have been commonly used as plasticizers and a variety of applications. Phthalate diesters have been shown to be developmental and reproductive toxicants. It is very difficult to exactly estimate the dose of dialkylated phthalates taken up by the general population because of environmental contamination. Urinary metabolites of phthalates enabled to estimate internal exposure. The objective of this study was quantitative determination of phthalate metabolites by LC/MS/MS with on-line cleanup method to analyze phthalate metabolites in Korean children's urine. We employed LC/MS/MS with on-line enrichment and column-switching techniques for this biological monitoring. Metabolites determined were 4 primary metabolites; MEHP, MnBP, MiBP, MEP and 2 secondary metabolites of DEHP; 5-OH-MEHP), 5-oxo-MEHP. We analyzed children's urine from 30 boys and 30 girls. The method detection limit of phthalate metabolites were 0.03 ng/mL for MEP, 1.05 ng/mL for MBP, 0.22 ng/mL for MEHP, 0.15 ng/mL for 5-OHMEHP and 0.16 ng/mL for 5-oxo-MEHP, respectively. Switching Column LC/MS/MS was proven to be a useful tool to determine metabolites of phthalate diesters in human urine. The correlation among phthalate metabolites was very high and statistically significant, except MEP. The children's age (months) was negatively correlated to the concentration of phthalate metabolites. The geometric mean concentration of phthalate metabolites (mg/g creatinine) in children's urine were 25.5 for MEP, 130.3 for MnBP, 56.8 for MiBP, 19.5 for MEHP, 85.6 for 5-OH-MEHP and 83.1 for 5-oxo-MEHP, respectively. Levels of estimated daily intake of parent phthalate compounds (${\mu}g$/kg bw/day) were 0.8 for DEP, 5.0 for DnBP, 1.9 for DiBP and $8.9{\sim}14.2$ for DEHP, respectively. Estimated daily intake for DEP and DiBP were lower than those of other studies but the value for DEHP was higher than that of other study.

Effects of Media and Temperatures on Micro Stem Cutting of Dendrobium nobile 'Hamana Lake Dream' × 'No. 55' in Vitro (Dendrobium nobile 'Hamana Lake Dream' × 'No.55'의 기내 줄기삽목에 미치는 배지의 종류와 온도의 영향)

  • Yoon, Jin-Young;Nam, Yu-Kyeong;Lee, Jong-Suk;Kim, Hyun-Jin
    • Journal of agriculture & life science
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    • v.44 no.3
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    • pp.23-30
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    • 2010
  • The optimal growth condition of in vitro stem cutting of Dendrobium nobile 'Hamana Lake Dream' ${\times}$ 'No. 55' was investigated. Among various media and their concentrations, MS media had better effect on the growth of micro stem cutting than Hyponex media in all concentration levels except stem length. The activated charcoal concentration in MS media showed different effects on number of stem and root, leaf length, and fresh weight: the most effective in the range of 0.1 to 1.0 g/L and barely effective above 2.0 g/L. Addition of agar 5 g/L, sucrose at 40 g/L, and peptone at 1 g/L to MS media increased significantly stem length, leaf width, and fresh weight, internode length and number of roots, and the number of stem and leaves. On the other hand, addition of gelite with any concentration had no effect on the growth of micro stem cutting compare to that of control. The optimal temperature for growth of micro stem cutting was $28^{\circ}C$. Under the same temperature, MS medium was better than Hyponex medium for the growth of stem. In addition, sucrose at 40 g/L was the most effective on growth at $28^{\circ}C$.

Simultaneous analysis of residual glucocorticoids in egg by LC/MS/MS (LC/MS/MS를 이용한 계란 중 잔류 글루코코티코이드의 동시분석)

  • Jang, Mi-Ae;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.326-335
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    • 2009
  • A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

Monitoring for β-agonist residues in raw meat in Seoul (식육에서 베타아고니스트계 약물 잔류 연구)

  • Choi, Yoon-Hwa;Kim, Mi-Ran;Kim, Young-Seob;Lee, Ju-Hyeong
    • Korean Journal of Veterinary Service
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    • v.40 no.1
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    • pp.79-82
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    • 2017
  • We investigated the residues of ${\beta}-agonist$ (zilpaterol, ractopamine and clenbuterol) using LC-MS/MS in raw meat in Seoul. The recoveries ranged between 76.7~89.9% in beef respectively. The limits of detection were $0.01{\sim}0.09{\mu}g/kg$ and the limits of quantification were $0.03{\sim}0.28{\mu}g/kg$ respectively. Residues of ${\beta}-agonist$ drugs which exceeded maximum residue limits (MRL) were not exceed in any of the 267 samples.

Determination of methamphetamine in the hair of Korean abuser by CG/MS (GC/MS에 의한 한국인의 모발중 Methamphetamine검출)

  • 유영찬;정희선;최화경
    • YAKHAK HOEJI
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    • v.37 no.4
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    • pp.356-361
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    • 1993
  • A sensitive method for the determination of methamphetamine(MA) and amphetamine(AM) in hair was developed by gas chromatography/mass spectrometry using stable isotope-labeled internal standards, amphetamine-d$_{5}$ and methamphetamine-d$_{5}$. Hair sample was washed with MeOH, incubated with MeOH(I% HCI) overnight at $37^{\circ}C$ while stirring and extracted using solid phase extraction column on a vacuum manifold. The extract obtained was pentafluoropropionated, and applied to GC/MS. The calibration curves of MA and AM were linear from 2.5 to 250 ng (r>0.99 for both). The limit of detection was 0.1 ng/mg in hair and cut-off level was set at 0.25 ng/mg for both. Hair samples of 27 MA abusers showed positive results in the range 0.7 to 106.8 ng/mg. AM, its metabolite, was detected in 20 out of 27 samples. The ratio of MA versus AM was 4.6~38.3 in specimens. Hair analysis for methamphetamine by GC/MS is an effective method for identifying long-term drug abusers.

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In vitro Micropropagation of Rosa hybrid L.

  • Kim Chang-Kil;Oh Jung-Youl;Jee Sun-Ok;Chung Jae-Dong
    • Journal of Plant Biotechnology
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    • v.5 no.2
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    • pp.115-119
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    • 2003
  • To determine the appropriate concentrations of nutrients and growth regulators for shoot proliferation and root initiation, several rose hybrid tea cultivars were cultured. Cultured shoot tips and lateral buds from different cultivars proliferated multiple shoots on Murashige and Skoog (MS) medium supplemented with 0 to 4 mg/L BA and 0 to 0.05 mg/L NAA. The ability of the explants to proliferate shoots and initiate roots was affected by genotype, the nodal position of explant, the strength of MS basal medium and growth regulators used. The buds nearest the apex exhibited the slowest rate of development. Most cultivars had the highest shoot proliferation when cultured on MS medium with 2 mg/L BA and 0.01 mg/L NAA, but the degree varied by cultivars. Root development was enhanced by lowering the concentration of MS salts.

Simultaneous determination of low molecular weight amines and quaternary ammonium ions by IC/ESI-MS

  • Jung, Joo-Young;Park, Han-Seok;Kim, Kang-Jin
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.255-260
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    • 2007
  • A new method for the simultaneous determination of low molecular weight amines and quaternary ammonium ions based on the separation by IC with a suppressor and the detection by MS with ESI has been developed. The method has been applied to the analysis of a mixture containing tetramethylammonium ion, tetraethylammonium ion, tetrapropylammonium ion, triethanolamine, trimethylamine and triethylamine. The constituents were separated by isocratic elution using an IonPac CS17 column, a cation-exchange column, and detected by conductivity and mass spectrometry. The newly developed method for the six components demonstrated that the repeatability in terms of relative standard deviation for three measurements was in the range of 0.1-0.5 %. The detection limits were between 0.2 and $0.9{\mu}g/mL$ by the IC/ESI-MS.

Pharmacoeconomics Evaluation of Morphine, MS Contin and Oxycodone in the Treatment of Cancer Pain

  • Zhang, Wen-Zhou;Yu, Wei-Jiang;Zhao, Xiu-Li;He, Bao-Xia
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.20
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    • pp.8797-8800
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    • 2014
  • Objective: To analyze cost-effectiveness of morphine, MS contin and oxycodone in the treatment of cancer pain, providing guidance for rational drug use in the clinic. Methods: Confirmed by histology, a total of 171 patients with various cancers who required analgesic treatment were selected and divided into 3 groups, 57 cases for each group, given morphine, MS contin and oxycodone, respectively. If there appeared a poor short-term effect or aggravated sudden pain during the treatment, a short-acting morphine injection was given and adverse reactions were processed by symptomatic treatment. The pain relief rate and adverse reactions of groups were observed and pharmacoeconomics evaluation was undertaken. Results: The pain relief rates with morphine, MS contin and oxycodone were 89.5%(51/57), 91.2%(52/57) and 93.0%(53/57), respectively, with no difference samong groups (${\chi}^2=4.4489$, P=0.6162). The occurrence rates of adverse reactions were 59.7%(34/57), 54.4%(31/57) and 43.9%(25/57), again with no significant variation (P>0.05). The ratios of cost-effectiveness (C/E) for the 3 groups were $14.6{\pm}7.21$, $15.0{\pm}7.44$ and $16.1{\pm}8.10$. When the price of 3 kinds of analgesics was reduced by 10%, the ratios of cost-effectiveness were $12.2{\pm}6.53$, ($13.4{\pm}6.08$ and $14.5{\pm}6.74$ but there was no differences when compared with before the price adjustment (t=1.86, P=0.0651; t=1.30, P=0.1948; t=1.17, P=0.2453). Conclusion: Morphine, MS contin and oxycodone give similar pain relief and adverse reaction rates but of all, morphine is the preferred drug for the treatment of cancer pain from the perspective of pharmacoeconomics.

Monitoring of 7 mycotoxins in pork (돼지고기에서 7종 mycotoxins 잔류실태 조사)

  • Kim, Yoen-Joo;Kim, Mi-Ran;Choi, Tae-Suk;Kim, Young-Seob;Lee, Ju-Hyoung
    • Korean Journal of Veterinary Service
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    • v.36 no.4
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    • pp.303-309
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    • 2013
  • This study was conducted to determine the content of 7 mycotoxins (aflatoxin $B_1$, $B_2$, $G_1$, $G_2$, $M_1$, ochratoxin A and zearalenone) using LC-MS/MS in pork available on the Korean markets. The analysis was carried out using following conditions; C18 column ($2.1{\times}100mm$, $1.7{\mu}m$), mobile phase composed of $H_2O$ (0.1 mM $NH_4Ac$ 0.01% HCOOH) : Methanol (0.1 mM $NH_4Ac$ 0.01% HCOOH), binary pump at a flow rate of 0.5 mL/min and $2{\mu}L$ of injection volume, MS/MS detector with ESI positive and negative mode. The quantication of mycotoxins was based on matrix-matched calibration curves with a correlation coefficient in excess of 0.99 for the 7 mycotoxins. The dectection limits were ranged 0.74~2.13 ng/g, with mean recoveries between 73.10~97.46% except aflatoxin $B_1$ (61.31%). We also monitored mycotoxin residues in 208 pork samples. The test results, mycotoxins were not found except one sample. Ochratoxin A in one sample of the test samples was detected below the quantification limit.

Determination of Adrenosterone and its Metabolites in Human Urine by LC/APCI/MS and GC/MS

  • Han, Eun-Jung;Yim, Ok-Kyoung;Beak, Sun-Young;Chung, Jae-Yeon;Lee, Ji-Hye;Kim, Jun-Gahn;Kim, Yun-Je
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1489-1496
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    • 2009
  • This study was done for the determination and excretion profile of adrenosterone and its metabolites in human urine using both liquid chromatography with atmospheric pressure chemical ionization mass spectrometry and gas chromatography with mass spectrometry. Adrenosterone and its two metabolites were detected in human urine after administration a healthy volunteer with 75 mg of adrenosterone. We found that adrenosterone-M1 ($C_{19}H_{26}O_3$) was a reduction and adrenosterone-M2 ($C_{19}H_{26}O_4$) was a hydroxylation at C-ring, which did not know the exact position of the C-ring. The adrenosterone parent was detected by GC/TOF-MS, but not detected by LC/APCI/MS because of low intensity. Adrenosterone and its two metabolites were excreted as their glucuronided fractions. The recovery of this method ranged from 100.7 to 118.4% and the reproducibility and accuracy test were 85.5 to 112.0% and 1.1 to 8.4%, respectively. The excretion studies showed that adrenosterone and its metabolites were detectable in human urine during a 48 h period after oral administration, with maximum level of excretion at 4.1 h. The glucuro-/sulfaconjugated ratio of adrenosterone, M1 and M2 was 0.73 ${\pm}$ 0.03, 0.96 ${\pm}$ 0.06 and 0.89 ${\pm}$ 0.03 (n = 6), respectively. The amounts of adrenosterone excreted in urine were 14.75 ng for 48 h. Also, the maximum level of androsterone and 11$\beta$-hydroxy androsterone, which were endogenous steroids, were reached 4.1 h after the oral administration of adrenosterone.