• Title/Summary/Keyword: LC MS/MS

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Simultaneous determination of seven major human cytochrome P450 activities using LC/MS/MS

  • Lee, Seung-Seok;Kim, Hae-Kyoung;Jin, Joon-Ki;Lee, Hye-Won;Kim, John;Lee, Hye-Suk
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.404.1-404.1
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    • 2002
  • A LC/MS/MS method for the simultaneous determination of the activities of seven major human drug-metabolizing cytochrome P450s (CYP3A4. CYP2D6. CYP2C9. CYP1A2, CYP2C19, CYP2A6. and CYP2C8) was developed. This method used an in vitro cocktail of specific substrates (midazolam. bufuralol. diclofenac, ethoxyresorufin. S-mephenYlOin. coumarin. and paclitaxel) and LC/MS/MS. The assay incubation time is 20 min and the analysis time is 8 min/sample. (omitted)

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LC-MS/MS-Based Comparative Investigation on Chemical Constituents of Six Aster Species Occurring in Korea

  • Kang, Kyo Bin;Lee, Dong Young;Sung, Sang Hyun
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.257-263
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    • 2021
  • Aster species (Asteraceae) are widely distributed edible and medicinal plants, known to contain various specialized metabolites including polyphenols and saponins. However, systemic analysis on the chemical profiles of these plants have rarely been made. Here we analyzed the phytochemical constituents in leaves of 6 Aster species occurring in Korea, A. ageratoides, A. altaicus var. uchiyamae, A. glehnii, A. hispidus, A. incisus, and A. yomena, by applying a LC-MS/MS-based untargeted metabolomics approach. The analysis revealed that A. ageratoides, A. hispidus, and A. yomena are relatively rich in saponins most of which are expected to be previously unknown.

Determination of Liraglutide in Rat Plasma Using Selective Liquid Chromatography-Tandem Mass Spectrometry

  • Younah Kim;Hyoje Jo;Yelim Lee;Soo Yeon Kang;Sangkyu Lee
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.141-146
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    • 2023
  • Liraglutide is a medication prescribed for the management of type 2 diabetes and chronic obesity. A simple, sensitive, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitative analysis of liraglutide in rat plasma. After a simple protein precipitation step, liraglutide was chromatographically separated using the ACQUITY Premier Peptide BEH C18 Column with mobile phases comprising 50% acetonitrile and 50% methanol, and water with 0.3% FA. Positive ion electrospray ionization in multiple reaction monitoring mode was used to achieve detection. Good linearity was observed in the 5-600 ng/mL concentration range (R2 > 0.99). Liraglutide had intra- and inter-day precision values of 2.13%-9.86% and 4.14%-8.36%, respectively. The accuracy ranged from -2.36% to 2.58%. The recovery and matrix effect were within acceptable limits. This selective LC-MS/MS method was used to study the pharmacokinetic properties of liraglutide after subcutaneous administration in rats.

Monitoring and Evaluation of Analytical Methods of Perchlorate with IC and LC/MS (IC와 LC-MS를 이용한 퍼클로레이트 분석 방법 비교 및 모니터링)

  • Kim, Hwa-Bin;Sim, Won-Jin;Kim, Min-Young;Oh, Jeong-Eun
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.1
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    • pp.37-44
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    • 2008
  • In this study, we tried to establish analysis methods of perchlorate with ion chromatography(IC) and liquid chromatography/mass spectrometry(LC/MS) and monitored perchlorate levels in various kinds of water and soil samples. The obtained method detection limit(MDL) of IC was 1 ppb and that of LC/MS was 0.005 ppb in water sample. We monitored the ground and spring water in Busan and the average perchlorate level in ground water was 0.031 $\pm$ 0.011 ppb and that of spring water was 0.013 $\pm$ 0.014 ppb. Wastewater samples were also examined and the levels of perchlorate ranged from 0.007 to 0.380 ppb. The perchlorate levels in all water samples investigated in this study were below the EPA guideline.

The Study on the Analysis Method of Tetrodotoxin in Puffer Fish (복어 중 테트로도톡신 분석법에 관한 연구)

  • Kang, Young-Woon;Lee, Yoon-Suk;Park, Sung-Kug;Seo, Jung-Heok;Kim, Mee-Hye
    • Journal of Food Hygiene and Safety
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    • v.27 no.1
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    • pp.37-41
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    • 2012
  • The current standard for testing tetrodotoxin (TTX) in foodstuffs is the mouse bioassay (MBA) in Korea as in many other countries. However, this test suffers from potential ethical concerns over the use of live animals. In addition, the mouse bioassay does not test for a specific toxin thus a sample resulting in mouse incapacitation would need further confirmatory testing to determine the exact source toxin (e.g., TTX, STX, brevotoxin, etc.). Furthermore, though the time of death is proportional to toxicity in this assay, the dynamic range for this proportional relationship is small thus many samples must be diluted and new mice be injected to yield a result that falls within the quantitative dynamic range. Therefore, in recent years, there have been many efforts in this field to develop alternative assays. High performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) has been emerged as one of the most promising options. A LC-MS-MS method involves solid-phase extraction (SPE) and followed by analysis using an electrospray in the positive ionization mode and multiple reactions monitoring (MRM). To adopt LC-MS-MS method as alternative standard for testing TTX, we performed a validation study for the quantification of TTX in puffer fish. This LC-MS-MS method showed good sensitivity as limits of detection (LOD) of $0.03{\sim}0.08{\mu}g/g$ and limits of quantification (LOQ) of $0.10{\sim}0.25{\mu}g/g$. The linearity ($r^2$) of tetrodotoxin were 0.9986~0.9997, the recovery were 80.9~103.0% and the relative standard deviations (RSD) were 4.3~13.0%. The correlation coefficient between the mouse bioassay and LC/MS/MS method was higher than 0.95.

LC-MS/MS Screening Method for Radical Scavenging Active Compounds in Extracts of Ulmus pumila Cortex (유근피 추출물의 radical 소거 활성 성분에 대한 LC-MS/MS 스크리닝 분석법)

  • Im, Do-Youn;Lee, Kyoung-In
    • Journal of Life Science
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    • v.30 no.11
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    • pp.956-964
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    • 2020
  • The radical scavenging activity measurement system linked with liquid chromatography (LC) is a useful tool for identifying the radical scavenging active compound in a sample composed of numerous compounds such as plant extracts. Using this system, DPPH and ABTS radical scavenging activity were measured on extracts of Ulmus pumila cortex, which is known as an herbal medicine with antioxidant activity. Mass spectrometry (MS) was performed on the identified radical scavenging active compounds to identify the four components estimated to be procyanidin B2, procyanidin B3, catechin-7-O-β-D-apiofuranoside, and catechin-5-O-β-D-apiofuranoside, respectively. In order to compare the relative contents between extract samples, multiple reaction monitoring (MRM) mode analysis conditions were set for the four compounds in order to examine the possibility of comparing the content of radical scavenging active compounds in Ulmus pumila cortex extract using LC-MS/MS. As a result of the relative content comparison, it was found that the higher the ethanol concentration of the extraction solvent, the higher the content of radical scavenging active compounds. As with the results of measuring the radical scavenging activity of each extract, it was confirmed that the content difference of three of the compounds (all except the compound estimated as procyanidin B3) was not significantly observed in the extracts with an ethanol concentration of 50% or more.

Sensitive Determination of Pinaverium Bromide in Human Plasma by LC-ESI-MS/MS : Applicability to Oral Bioavailability Determination (LC-ESI-MS/MS를 이용한 생체시료 중 브롬화피나베리움의 고감도 분석 및 이를 이용한 생체이용률 평가)

  • Park, Seok;Lee, Ye-Rie;Kim, Ho-Hyun;Lee, Hee-Joo;Kim, Yoon-Gyoon;Youm, Jeong-Rok;Han, Sang-Beom
    • Journal of Pharmaceutical Investigation
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    • v.34 no.6
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    • pp.513-519
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    • 2004
  • A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

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
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    • v.31 no.1
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    • pp.15-20
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    • 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%.

Evaluation of LC/MS and LC/UVD(EPA-631) Methods in Determination of Benomyl Concentration in Water Samples (LC/MS법 및 LC/UVD(EPA-631)를 이용한 수계 중 Benomyl의 분석법 평가)

  • Kim, Kee D.;Choi, Won Gyu;Seo, Yong Chan;Park, Byung Hwang;Choi, Hye Kyung
    • Journal of the Korean Chemical Society
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    • v.45 no.1
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    • pp.40-44
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    • 2001
  • Benomyl, one of the known endocrine disrupting chemicals, was analyzed to understand the its fate in water. Benomyl analysis process in water sample include the following sequential steps. Hydrolysis of benomyl into carbendazim, solvent extraction, concentration, and the concentration of final carbendazim solution was determined by LC/MS (TOF). Recoveries of the spiked samples were good with the range of 80.6 to 118.6% and the MDL was 1,600 times lower than that of LC/UVD method. The use of LC/MS (TOF) successfully eliminated the positive error incurred by interferencing materials in the matrix.

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