• Title/Summary/Keyword: LC-MS-MS

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Monitoring of Veterinary Drug Residues in Cultured Fishery Products in Chungcheongnam-do Province (충남지역에서 생산되는 양식수산물의 잔류 동물용의약품 모니터링)

  • Lee, Kang-Bum;Kim, Nam-Woo;Kim, Dong-Uk;Sin, Myeong-Hee;Lee, Mi-Young
    • Journal of Food Hygiene and Safety
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    • v.35 no.5
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    • pp.447-451
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    • 2020
  • For this study, we conducted a simultaneous multiresidue analysis of veterinary drugs in cultured fishery products in Chungnam Province in 2018. A total of 115 fishery product samples were obtained from fish farms and fishery production sites located in the province. In all, 29 residual veterinary drugs in the samples were analyzed using a validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. As a result, veterinary drug residues were only detected in a small number of the 106 samples (92.2%), and the detection rate was 7.8% (9 of 115 samples). The amounts were also below maximum residual limit (MRL) for fishery products, although one sample exceeded the MRL allowed by the Ministry of Food and Drug Safety and was detected in loach. The nine residual veterinary drugs were detected in 8 samples: loach, eel, catfish, freshwater bream, flatfish, rockfish and shrimp. The detected veterinary drugs were oxolinic acid, enrofloxacin, ciprofloxacin, sulfadiazine, flumequine and oxytetracycline. The most frequently detected antibiotic was oxolinic acid, and enrofloxacin exceeded the MRL in loach sample. Residues of most veterinary drugs were either not detected or were below the MRL, and while the status of fishery products is seen as safe overall, current surveillance efforts over veterinary drugs should be continued.

A Case of Short-chain Acyl-CoA Dehydrogenase Deficiency Detected by Newborn Screening

  • Park, Kyungwon;Ko, Jung Min;Jung, Goun;Lee, Hee Chul;Yoon, So Young;Ko, Sun Young;Lee, Yeon Kyung;Shin, Son Moon;Park, Sung Won
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.15 no.1
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    • pp.40-43
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    • 2015
  • Short-chain acyl-CoA dehydrogenase (SCAD) deficiency is an autosomal recessive mitochondrial disorder of fatty acid oxidation associated with mutations in the ACADS gene. While patients diagnosed clinically have a variable clinical presentation, patients diagnosed by newborn screening are largely asymptomatic. We describe here the case of a 1-year-old male patient who was detected by newborn screening and diagnosed as SCAD deficiency. Spectrometric screening for inborn errors of metabolism at 72hrs after birth showed elevated butyrylcarnitine (C4) level of 1.69 mol/L (normal, <0.83 mol/L), C4/C2 ration of 0.26 (normal, <0.09), C5DC+C60H level of 39 mol/L (normal, <0.28 mol/L), and C5DC/C8 ration of 7.36 (normal, <4.45). The follow-up testing at 18 days of age were performed: liquid chromatography tandem mass spectrometry (LC-MS/MS), urine organic acids, and quantitative acylcarnitine profile. C4 carnitine was elevated as 0.91; urine organic acid analysis showed elevated ethylmalonic acid as 62.87 nmol/molCr (normal, <6.5), methylsuccinate 6.81 nmol/molCr (normal, not detected). Sequence analysis of ACADS revealed a homozygous missense mutation, c.164C>T (p.Pro55Leu). He is growing well and no episodes of seizures or growth retardation had occurred.

Determination of radiolysis products in Tri-Octyl Amine by high performance liquid chromatography-mass spectrometer (HPLC-MS에 의한 Tri-Octyl Amine(TOA)의 방사선 분해산물 정량)

  • Yang, Han-Beom;Lee, Eil-Hee;Moon, Hyung-Sil
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.201-205
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    • 2005
  • Tri-octyl amine (TOA) is used in solvent extraction process for radioactive waste. This compound may be degraded to di-octyl amine (DOA), mono-octyl amine (MOA) by radioactive materials. Amount of TOA, DOA and MOA in TOA must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for TOA, DOA and MOA are studied with Phenomenex LUNA-$C_{18}$ ($4.6mm{\times}25cm$) analytical column and $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) eluent by liquid chromatography. Optimum condition for these compounds is $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) = 85 : 15 ratio. TOA, DOA and MOA compounds is well separated within 20 minute. Dynamic range is $30{\sim}160{\mu}g/mL$ for TOA, $5{\sim}100{\mu}g/mL$ for DOA and $0.1{\sim}5{\mu}g/mL$ for MOA, respectively. The detection limit are $0.1{\mu}g/mL$ for TOA, $1{\mu}g/mL$ for DOA (in SCAN mode) and $0.1{\mu}g/mL$ for MOA (in SIM mode) in this system with $20{\mu}L$ sample loop.

Development and Validation of a Simultaneous Analytical Method for the Detection of Mefentrifluconazole and Triticonazole Fungicide in Agricultural Crops (농산물 중 메펜트리플루코나졸 및 트리티코나졸 살균제의 동시 분석법 개발 및 검증)

  • Park, Ji-Su;Lee, Han Sol;Lee, Su Jung;Shin, Hye-Sun;Shim, Jae-Han;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Korean Journal of Environmental Agriculture
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    • v.39 no.2
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    • pp.130-137
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    • 2020
  • BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r2>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

Pharmacokinetics of amoxicillin after intramuscular injection at different temperatures to cultured olive flounder, Paralichthys olivaceus (Amoxicillin의 근육투여에 따른 수온별 넙치 체내 약동학적 특성)

  • Kim, Ji-Soo;Lee, Ji-Hoon;Lee, Soo-Jin;Park, Kwan-Ha
    • Journal of fish pathology
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    • v.28 no.1
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    • pp.43-51
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    • 2015
  • The pharmacokinetic properties and residue levels of amoxicillin (AMOX) were studied after intramuscular injection to cultured olive flounders ($100{\pm}50g$), Paralichthys olivaceus. For pharmacokinetic studies, AMOX of 20 to 80 mg/kg body weight was administered at $17{\pm}2^{\circ}C$ or $22{\pm}2^{\circ}C$ and AMOX concentrations were determined in plasma, the liver, and the kidney by HPLC-UVD. Plasma samples were assessed at 0.25, 0.5, 1, 3, 6, 12, 24, 48, 72, 96, 168 hours post-dose, whereas liver and kidney concentrations were measured at 0.25 to 48 hours post-dose. The kinetic profiles of AMOX were analyzed by fitting to a 2-compartmental model with PKSolver program. The following parameters were obtained for a single dosage of 20, 40 and 80 mg/kg of body weight at $22^{\circ}C$ and 20 and 40 mg/kg of body weight at $17^{\circ}C$ in plasma, liver and kidney, respectively: $C_{max}$ (the peak concentration)= $27.23-257.36{\mu}g/m{\ell}$, $5.49-41.65{\mu}g/g$, $16.75-129.31{\mu}g/g$; $t_{max}$ (the time for peak concentration)= 0.05-0.91, 1.36-3.28, 1.95-4.49 h. For residue studies, AMOX of 40 and 400mg/kg was administered, and muscle samples were taken at 2, 5, 7, 14 and 21 days post-dose. The residueof AMOX in the muscle were found under the MRLs (maximum residue levels) within 7 days for the two doses.

Screening of Potential Anticancer Compounds from Marketed Drugs: Aripiprazole, Haloperidol, Miconazole, and Terfenadine Inhibit Cytochrome P450 2J2 (시판 약물의 시토크롬 2J2 약물대사효소 저해능 탐색)

  • Liu, Kwang-Hyeon
    • Journal of Life Science
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    • v.21 no.11
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    • pp.1558-1564
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    • 2011
  • Cytochrome P450 2J2 (CYP2J2) plays important roles in the metabolism of endogenous metabolites such as arachidonic acid as well as therapeutic drugs. CYP2J2 is overexpressed in human cancer tissues and cancer cell lines, as well as in epoxyeicosatrienoic acids (EETs) and CYP2J2-mediated metabolites, and prevent apoptosis of cancer cells. This study aimed to screen marketed drugs for inhibitory potential on CYP2J2 isoforms using human liver microsomes. The initial screen isolated 4 compounds, from 120 marketed drugs, that inhibited the CYP2J2-mediated astemizole O-demethylation more than 50% in the following the order: haloperidol (75%) > terfenadine (56%) > aripiprazole (55%) > miconazole (52%). Miconazole strongly inhibited CYP2J2-mediated ebastine hydroxylation ($IC_{50}$=11.2 ${\mu}M$) and terfenadine hydroxylation ($IC_{50}$=2.2 ${\mu}M$), and terfenadine also inhibited CYP2J2-mediated ebastine hydroxylation ($IC_{50}$=13.6 ${\mu}M$) in a dose dependent manner. The present data suggest that these drugs are potential candidates for further evaluation for their anti-cancer activities.

Inhibition of Drug-metabolizing Enzyme and Drug Transporter by Major Components of Phellodendri cortex (황백의 주요 구성 화합물에 의한 약물대사효소 및 약물수송단백 저해능 평가)

  • Ku, Hei-Young;Kim, Hyunmi;Shon, Ji-Hong;Liu, Kwang-Hyeon
    • Journal of Marine Bioscience and Biotechnology
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    • v.1 no.3
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    • pp.213-217
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    • 2006
  • We evaluated the potential of major components of Phellodendri cortex to inhibit the activities of CYP2D6 and p-glycoprotein. The abilities of berberine, palmatine, limonin, and rutaecarpine to inhibit CYP2D6-mediated dextromethorphan O-demethylation and calcein AM accumulation were tested using human liver microsomes and L-MDR1 cell, respectively. Berberine strongly inhibited CYP2D6 isoform activity, whereas limonin and reuaecarpine did not. The $IC_{50}$ value of berberine was reduced after preincubation with microsomes in the presence of NADPH generating system, suggesting that berberine is a mechanism based inhibitor. In addition, all chemicals tested, didn't show inhibitory effect on p-glycoprotein activity. These results suggest that berberine has potential to inhibit CYP2D6 activity in vitro. Therefore, in vivo studies investigating the interactions between berberine and CYP2D6 substrates are necessary to determine whether inhibition of CYP2D6 activity by berberine is clinically relevant.

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Antioxidant Activity and Nutrient Content of Ethanol and Hot-Water Extracts of Citrus unshiu Pomace (감귤박 에탄올추출물과 열수추출물의 영양성분 및 항산화 활성)

  • Song, Yeonwoo;Moon, Keun Sik;Kim Cho, Somi
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.9
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    • pp.1345-1350
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    • 2013
  • The objective of this study was to evaluate the effect of extraction methods on the antioxidant activity of Citrus unshiu pomace. For this purpose, two kinds of citrus pomace (CP)s, whole fruit CP and pulp CP, were used for preparing the extracts with hot water or 70% ethanol. It is well-known fact that whole fruit CP has more calories and carbohydrates, although moisture content is higher in pulp CP. Further, whole fruit CP extracts have higher levels of total phenolic contents compared to CP extracts. In addition, DPPH and alkyl radical scavenging activities were also higher in whole fruit CP, especially in ethanolic extracts. Our results based on liquid chromatography-mass spectrometer showed that 70% ethanolic extract of whole fruit CP has the maximum levels of nobiletin and tangeretin contents. The levels of naringin, which is known as an antioxidant flavonoid, was determined only in the 70% ethanolic extract of whole fruit CP. This result, however, is consistent with the observed DPPH and alkyl radical scavenging activities. We had also performed a gas chromatography analysis that showed all the four extracts contained the compound hydroxymethyl furfural. Significantly, this compound has been reported to have antioxidant activity. Taken together, findings of this study indicate that ethanolic extraction of whole fruit CP is a good source of antioxidant compounds and hence the same could be utilized as an important method to obtain such beneficial compounds on an industrial scale.

Antimelanogenic Effect and Whitening of Anthocyanin Rich Fraction from Seeds of Liriope platyphylla (맥문동 종실 안토시아닌 분획물의 멜라닌 생성 억제 및 미백 효과)

  • Choung, Myoung Gun;Hwang, Young Sun;Kim, Gi Ppeum;Ahn, Kyung Geun;Shim, Hoon Seob;Hong, Seung Beom;Choi, Jae Hoo;Yu, Chang Yeon;Chung, Ill Min;Kim, Seung Hyun;Lim, Jung Dae
    • Korean Journal of Medicinal Crop Science
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    • v.21 no.5
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    • pp.361-371
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    • 2013
  • This study was performed to determine the antimelanogenic effect and tyrosinase inhibitory activities of anthocyanin rich fraction (AN-SLP) from Liriope platyphylla Wang et Tang seeds. Anthocyanins isolated from L. platyphylla seeds revealed the presence of four major anthocyanin components, which were tentatively identified as delphinidin-3-Oglucoside, delphinidin-3-O-rutinoside, petunidin-3-O-rutinoside, and malvidin-3-O-rutinoside using semipreparative HPLC, $^1H$-NMR, $^{13}C$ NMR, FAB-MS and LC/ES-MS. The inhibitory effect of AN-SLP on tyrosinase activity was studied using in vitro (against mushroom tyrosinase) and ex vivo (against B16 melanoma cell tyrosinase) models. Cellular tyrosinase activity was decreased by AN-SLP treatment in B 16 melanoma cells through dose dependent manner, but AN-SLP did not inhibit mushroom tyrosinase and L-DOPA oxidation directly. AN-SLP showed melanin inhibition by 53.2% at 50 ${\mu}g/m{\ell}$ which was 0.7 times more efficient than the antimelanogenic effect of commercial arbutin and kojic acid (36.5%) also did not show cell toxicity. Additionally, AN-SLP inhibited the activity of ${\alpha}$-glucosidase and the glycosylation of tyrosinase in melanoma cell. The resulting unsaturated glycosylation of tyrosinase makes it unstable and disturb correct transportation. From theses results, we conclude that AN-SLP could be used as anti-melanogenic agent for skin whitening.

Screening for inhibitory effect on nine CYP isoforms by 20 herbal medications (고속 스크리닝 기법을 이용한 한약제제의 cytochrome P45O 저해능 탐색)

  • Kim, Hyun-Mi;Liu, Kwang-Hyeon
    • Journal of Life Science
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    • v.17 no.3 s.83
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    • pp.334-339
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    • 2007
  • We evaluated the potential of 20 herbal medications (HMs), commonly used in Korea, to inhibit the catalytic activities of several cytochrome P450 (CYP) isoforms. The abilities of 500 ${\mu}g/ml$ of aqueous extracts of 20 HMs to inhibit phenacetin O-deethylation (CYP1A2), coumarin 6-hydroxylation (CYP2A6), bupropion hydroxylation (CYP2B6), rosiglitazone hydroxylation (CYP2C8), tolbutamide 4-methylhydroxylation (CYP2C9), S-mephenytoin 4'-hydroxylation (CYP2C19), dextromethorphan O-demethylation (CYP2D6), chlorzoxazone 6-hydroxylation (CYP2E1), and midazolam 1'-hydroxylation (CYP3A) were tested using human liver microsomes. The HMs Woohwangcheongsimwon suspension and Hwanglyeonhaedok-Tang strongly inhibited CYP2B6 and CYP2D6 isoform activity, respectively. These results suggest that some of the HMs used in Korea have potential to inhibit CYP isoforms in vitro. Although the plasma concentrations of the active constituents of the HMs were not determined, some herbs could cause clinically significant interactions because the usual doses of those individual herbs are several grams of freeze-dried extracts.