• 제목/요약/키워드: Liquid Chromatography-tandem Mass Spectrometry

검색결과 400건 처리시간 0.026초

이팩사® XR서방캅셀(벤라팍신, 75 mg)에 대한 벤팍신®OR서방정의 생물학적동등성 (Bioequivalence of Efexor® XR capsule to Venfaxine® OR tablet (Venlafaxine 75 mg))

  • 디펜드라 쿠마 아리얼;오수연;조종태;김형건;김윤균
    • Journal of Pharmaceutical Investigation
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    • 제37권6호
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    • pp.397-402
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    • 2007
  • To evaluate the bioequivalence of two venlafaxine formulations, a standard 2-way randomized cross-over study was conducted in twenty-four healthy male Korean volunteers. A single oral dose of 75 mg of test formulation Venfaxine $OR^{(R)}$ (tablet) or reference formulation Efexor $XR^{(R)}$ (capsule) was administered with one-week washout period. Plasma concentrations of venlafaxine were assayed for over a period of 72 hours with a well validated method using liquid chromatography coupled to tandem mass spectrometry (LC-MS-MS). The $mean{\pm}S.D$. of maximum concentration $(C_{max})$ and elimination half-life $(t_{1/2})$ were $64.7{\pm}28.5$ ng/mL, $9.2{\pm}3.0$ h, and $67.2{\pm}30.2$ ng/mL, $9.9{\pm}3.5$ h for test and reference formulations, respectively. Time to reach maximum concentration $(T_{max})$ expressed in median value (range), for the test and the reference, were 10 h (6-14) and 8h (4-12), respectively. Similarly, area under the plasma concentration-time curve, from time zero to last sampling time $(AUC_t)$ and from time zero to time infinity $(AUC_{inf})$, for test and reference formulations were $1185{\pm}755$, $1326{\pm}896$ and $1124{\pm}737$, $1185{\pm}755$ $ng{\cdot}h/mL$, respectively. The parametric 90% confidence intervals on the mean of the differences between the two formulations (test-reference) of the log transformed values of $AUC_t$, and $C_{max}$ were 0.9630 to 1.1383 and 0.8650 to 1.0446, respectively. The overall results indicate that the two formulations are bioequivalent and can be prescribe interchangeably.

식품 중 발기부전치료제 및 사용금지 성분 모니터링 (Monitoring of illegal compounds and prohibited natural ingredients in foods)

  • 윤지숙;최장덕;권기성;조천호
    • 한국식품과학회지
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    • 제48권5호
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    • pp.405-412
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    • 2016
  • 성기능개선, 원기증강 등에 효과가 있는 것으로 판매되고 있는 식품 등에서 발기부전치료제 및 그 유사물질 등이 불법적으로 혼입되어 검출되고 있다. 이들 부정물질이 혼입된 불량식품은 안전성과 유효성이 입증되지 않았기 때문에 국민건강을 위협할 수 있다. 그러므로 본 연구에서는 식품과 가짜 발기부전치료제에 불법 혼입된 부정물질을 모니터링하기 위하여, 해외 인터넷 사이트와 오프라인 매장에서 성기능개선, 원기증진을 표방하는 식품과 최음제, 가짜 발기부전치료제 161건을 구입하였다. 시험방법의 유효성 검증을 위하여 선택성, 직선성, 검출한계, 정량한계, 정확성, 정밀성을 검토하였다. LC-PDA와 LC-MS/MS를 이용하여 부정물질 54종을 동시분석한 결과, 48건의 시료에서 7종의 부정물질(요힘빈, 이카린, 실데나필, 타다라필, 클로로프레타다라필, 데메틸실데나필, 디메틸치오실데나필)이 검출되었다. 성기능개선이나 최음제로 판매되는 제품에는 부정물질이 혼입될 가능성이 있으므로, 이들 제품을 구입할 때는 각별한 주의가 필요하다.

식품 중 부정 혼입된 비만치료제 및 사용금지 성분 실태조사 (Screening of anti-obesity drugs, their analogues and prohibited ingredients in slimming foods)

  • 윤지숙;최장덕;권기성;조천호
    • 한국식품과학회지
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    • 제48권5호
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    • pp.424-429
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    • 2016
  • 비만은 전세계적으로 심각한 문제로 인식되고 있다. 최근 체중감소와 유지를 위한 다이어트제품에 비만치료제와 그 유사물질, 사용금지 성분들이 발견되고 있다. 정부의 감시를 피하기 위하여, 비만치료제의 화학구조를 일부 변형시킨 유사물질이 지속적으로 합성되고 있다. 부정물질이 혼입된 다이어트식품을 신속하게 검사하기 위하여, 국내에서 판매되는 제품과 해외 인터넷 사이트에서 128건의 다이어트제품을 구매하였으며, HPLC-PDA와 LC-MS/MS로 21종의 부정물질을 동시분석하였다. 시험법의 유효성 검증은 선택성, 직선성, 검출한계, 정량한계, 정확성, 정밀성을 검토하였다. 분석결과 31건의 시료에서 부정물질이 검출되었으며, 검출수준은 시부트라민 9.9-135.3 mg/g, 요힘빈 0.2-17.5 mg/g, 이카린 1.8 mg/g이었다. 본 연구의 부정물질 분석법은 간단하면서도 신속한 분석법으로, 식품안전관리를 위한 기초자료로 활용될 수 있을 것으로 사료된다.

지방질다당류로 자극한 RAW 264.7 세포에서 청도반시 땡감 에틸 아세테이트 분획물의 항염증 효과 (Anti-inflammatory effects of ethyl acetate fraction of unripe astringent persimmon (Diospyros kaki Thunb. cv. Cheongdo-Bansi) on lipopolysaccharide-stimulated RAW 264.7 cells)

  • 박예빈;정하람;이승환;김태완;김대옥
    • 한국식품과학회지
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    • 제51권1호
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    • pp.90-96
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    • 2019
  • 본 연구에서는 적과한 청도반시 땡감을 40% (v/v) 에탄올-물 혼합 용액으로 추출하고, 이 추출물을 액체-액체 추출법으로 5개 분획물(노말-헥세인, 클로로폼, 에틸 아세테이트, 노말-뷰탄올, 물)을 얻었다. 5개 분획물 중에서 에틸 아세테이트 분획물이 총 페놀 함량, 총 플라보노이드 함량 및 산화방지능이 가장 높았다. 에틸 아세테이트 분획물은 지방질다당류로 자극한 RAW 264.7 세포에서 산화 질소, IL-6, 산화 스트레스를 감소시켰다. UPLC-ESI-MS/MS를 이용하여 땡감 에틸 아세테이트 분획물에서 페놀 화합물로 갈산, 프로토카테츄산, 4-하이드록시벤조산, 쿼서틴-3-O-글루코사이드, 파라-쿠마르산, 쿼서틴을 동정하였다. 본 연구를 통해서 적과 과정에서 부산물로 버려지는 청도반시 땡감이 산화방지능 및 항염증 효과를 보유한 기능성 소재로서 활용될 가능성을 제시하였다. 그러나 향후 적과한 청도반시 땡감의 산화방지능에 기반한 항염증 효과를 좀 더 명확하게 밝히기 위해서는 청도반시 땡감에 존재하는 개별 생리활성물질의 정량 분석 및 항염증에 대한 분자생물학적 메커니즘을 규명할 필요가 있다.

Uptake and Distribution of Bisphenol A and Its Metabolites in Lettuce Grown in Sandy Loam and Loam Soil

  • Cho, Il Kyu;Jeon, Yong-Bae;Oh, Young Goun;Rahman, Md. Musfiqur;Kim, Won-Il;Lee, Young-Deuk
    • 한국환경농학회지
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    • 제39권4호
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    • pp.375-383
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    • 2020
  • BACKGROUND: Bisphenol A (BPA) is a chemical widely used in polycarbonate plastics, epoxy resins. BPA is an endocrine disruptor. Residue of BPA in agricultural environments is a major concern. The objective of this study was to understand the characteristics of the uptake and distribution of BPA and its metabolites introduced into the agricultural environment to crops, and to use it as basic data for further research on reduction of BPA in agricultural products. METHODS AND RESULTS: This study established the analysis method of BPA and its metabolites in soil and crops, and estimated the intake of BPA and its metabolites from lettuce (Lactuca sativa) grown in sandy loam and loam soil, which are representative soils in Korea. The two major metabolites of BPA were 4-hydroxyacetophenone (4-HAP) and 4-hydroxybenzoic acid (4-HBA). BPA, 4-HAP and 4-HBA have been analyzed by using liquid chromatography tandem mass spectrometry (LC-MS/MS). These substances were detected in sandy loam and loam soil, indicating that certain portions of BPA were converted to 4-HAP and 4-HBA in the soil; however, it was observed that only 4-HBA migrated to lettuce through the roots into crops. CONCLUSION: The uptake residues showed the BPA and 4-HAP were not detected in lettuces grown on sandy loam (SL) and loam (L) soil treatments that were applied with of 10 ng/g, 50 ng/kg and 500 ng/g of BPA. However, the 4-HBA was detected at the level of 7 ng/g and 11 ng/g in the lettuce grown in sandy loam and loam soil that were treated with the 500 ng/g of BPA, respectively, while the 8 ng/g of 4-HBA was measured in the lettuce cultivated in the loam that was treated with 100 ng/g of BPA. This result presents that the BPA persisting in the soil of the pot was absorbed through the lettuce roots and then distributed in the lettuce leaves at the converted form of 4-HBA, what is the oxidative metabolite of BPA.

Gintonin facilitates brain delivery of donepezil, a therapeutic drug for Alzheimer disease, through lysophosphatidic acid 1/3 and vascular endothelial growth factor receptors

  • Choi, Sun-Hye;Lee, Na-Eun;Cho, Hee-Jung;Lee, Ra Mi;Rhim, Hyewhon;Kim, Hyoung-Chun;Han, Mun;Lee, Eun-Hee;Park, Juyoung;Kim, Jeong Nam;Kim, Byung Joo;Nah, Seung-Yeol
    • Journal of Ginseng Research
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    • 제45권2호
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    • pp.264-272
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    • 2021
  • Background: Gintonin is a ginseng-derived exogenous G-protein-coupled lysophosphatidic acid (LPA) receptor ligand, which exhibits in vitro and in vivo functions against Alzheimer disease (AD) through lysophosphatidic acid 1/3 receptors. A recent study demonstrated that systemic treatment with gintonin enhances paracellular permeability of the blood-brain barrier (BBB) through the LPA1/3 receptor. However, little is known about whether gintonin can enhance brain delivery of donepezil (DPZ) (Aricept), which is a representative cognition-improving drug used in AD clinics. In the present study, we examined whether systemic administration of gintonin can stimulate brain delivery of DPZ. Methods: We administered gintonin and DPZ alone or coadministered gintonin with DPZ intravenously or orally to rats. Then we collected the cerebral spinal fluid (CSF) and serum and determined the DPZ concentration through liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Results: Intravenous, but not oral, coadministration of gintonin with DPZ increased the CSF concentration of DPZ in a concentration- and time-dependent manner. Gintonin-mediated enhancement of brain delivery of DPZ was blocked by Ki16425, a LPA1/3 receptor antagonist. Coadministration of vascular endothelial growth factor (VEGF) + gintonin with DPZ similarly increased CSF DPZ concentration. However, gintonin-mediated enhancement of brain delivery of DPZ was blocked by axitinip, a VEGF receptor antagonist. Mannitol, a BBB disrupting agent that increases the BBB permeability, enhanced gintonin-mediated enhancement of brain delivery of DPZ. Conclusions: We found that intravenous, but not oral, coadministration of gintonin facilitates brain delivery of DPZ from plasma via LPA1/3 and VEGF receptors. Gintonin is a potential candidate as a ginseng-derived novel agent for the brain delivery of DPZ for treatment of patients with AD.

양식어류 중 Ethoxyquin과 Ethoxyquin dimer의 잔류분석 및 위해평가 (Residue analysis and risk assessment of ethoxyquin and ethoxyquin dimer in farmed fish)

  • 최영희;고숙경;류승희;진영희;곽재은;이명숙;김복순;황인숙
    • 한국식품과학회지
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    • 제53권3호
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    • pp.239-244
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    • 2021
  • 서울시내 도매시장 및 재래시장에서 판매되는 양식어류 288건에 대해 에톡시퀸과 에톡시퀸 다이머의 잔류량을 LC-MS/MS로 분석하고 위해평가를 수행하였다. 에톡시퀸과 에톡시퀸 다이머의 검출 범위(검출률)는 각각 민물어류의 경우 0.005-0.309 mg/kg (15.7%), 0.002-2.828 mg/kg (90.0%), 해양어류의 경우 0.009-0.024 mg/kg (2.5%), 0.001-1.790 (63.3%)로 나타났다. 에톡시퀸은 민물장어, 미꾸라지, 동자개, 넙치에서만 검출된 반면 에톡시퀸 다이머는 민물어류 5종 및 해양어류 6종에서 검출되었다. 식이노출평가를 위해 ADI와 EDI를 이용하여 미꾸라지, 민물장어, 돔, 넙치 우럭을 대상으로 HI를 계산한 결과 0.002-0.301%로 나타났다. 본 연구 결과, 10건의 양식 어류가 잔류물질 허용기준 1.0 mg/kg을 초과하였지만, 인체 건강에 잠재적인 위해성이 매우 적은 것으로 나타났다. 하지만 이번 연구 결과는 식품에 허가되어 있지 않는 항산화제인 에톡시퀸 및 에톡시퀸 다이머가 사료로부터 양식어류에 이행되어 인간에게 노출되고 있음을 과학적으로 입증할 수 있는 근거 자료가 되었다.

Plasma metabolites associated with physiological and biochemical indexes indicate the effect of caging stress on mallard ducks (Anas platyrhynchos)

  • Zheng, Chao;Wu, Yan;Liang, Zhen Hua;Pi, Jin Song;Cheng, Shi Bin;Wei, Wen Zhuo;Liu, Jing Bo;Lu, Li Zhi;Zhang, Hao
    • Animal Bioscience
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    • 제35권2호
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    • pp.224-235
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    • 2022
  • Objective: Cage rearing has critical implications for the laying duck industry because it is convenient for feeding and management. However, caging stress is a type of chronic stress that induces maladaptation. Environmental stress responses have been extensively studied, but no detailed information is available about the comprehensive changes in plasma metabolites at different stages of caging stress in ducks. We designed this experiment to analyze the effects of caging stress on performance parameters and oxidative stress indexes in ducks. Methods: Liquid chromatography tandem mass spectrometry (LC/MS-MS) was used to determine the changes in metabolites in duck plasma at 5 (CR5), 10 (CR10), and 15 (CR15) days after cage rearing and traditional breeding (TB). The associated pathways of differentially altered metabolites were analyzed using Kyoto encyclopedia of genes and genomes (KEGG) database. Results: The results of this study indicate that caging stress decreased performance parameters, and the plasma total superoxide dismutase levels were increased in the CR10 group compared with the other groups. In addition, 1,431 metabolites were detected. Compared with the TB group, 134, 381, and 190 differentially produced metabolites were identified in the CR5, CR10, and CR15 groups, respectively. The results of principal component analysis (PCA) show that the selected components sufficiently distinguish the TB group and CR10 group. KEGG analysis results revealed that the differentially altered metabolites in duck plasma from the CR5 and TB groups were mainly associated with ovarian steroidogenesis, biosynthesis of unsaturated fatty acids, and phenylalanine metabolism. Conclusion: In this study, the production performance, blood indexes, number of metabolites and PCA were compared to determine effect of the caging stress stage on ducks. We inferred from the experimental results that caging-stressed ducks were in the sensitive phase in the first 5 days after caging, caging for approximately 10 days was an important transition phase, and then the duck continually adapted.

LC-MS/MS를 이용한 축·수산물 중 β-agonist계 시험법 개발 및 검증 (Development and Validation of an Analytical Method for β-Agonists in Livestock and Fishery Products Using LC-MS/MS)

  • 이태호;김유라;박수정;김지영;최장덕;문귀임
    • 한국환경농학회지
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    • 제41권2호
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    • pp.135-151
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    • 2022
  • BACKGROUND: The β-agonists known as phenyl ethanolamine derivatives have a conjugated aromatic ring with amino group. They are used as tocolytic agents and bronchodilator to human and animal generally, and some of them are used as growth promoters to livestock. METHODS AND RESULTS: β-agonists in samples were extracted by 0.4 N perchloric acid and ethyl acetate. The target compounds were analyzed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS). Validation of method was performed according to CODEX guidelines (CAC/GL-71). The matrix matched calibration gave correlation coefficients>0.98, and the obtained recoveries were in the range of 62.0-109.8%, with relative standard deviation ≤ 20.1%. In addition, a survey was performed to inspect any residual β-agonist from 100 samples of livestock and fishery products and ractopamine was detected in one of the 100 samples. CONCLUSION(S): In this study, we established the analytical method for β-agonists through using the expanded target compounds and samples. And we anticipate that the established method would be used for analysis to determine veterinary drug residues in livestock and fishery products.

케일 중 살충제 Flubendiamide의 잔류 특성 (Residual characteristics of insecticide flubendiamide in kale)

  • 김현진;황규원;선정훈;이태현;정경수;문준관
    • Journal of Applied Biological Chemistry
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    • 제65권3호
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    • pp.173-181
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    • 2022
  • 본 연구는 케일 중 flubendiamide의 잔류 특성을 조사하여 생산단계 잔류허용기준(PHRL, Pre-Harvest Residue Limit)을 설정하고자 하였으며, 세척용매 및 세척방법에 따른 제거효율을 알아보기 위해 수행되었다. 포장 시험은 포장 1 (경기도 안성시)과 포장 2(경기도 이천시)의 시설재배 하우스 두 곳에서 실시하였다. 농약의 안전사용기준에 따라 10일간격 2회 살포하고 0 (2시간 후), 1, 2, 3, 5, 7, 10일차에 수확하였다. Flubendiamide의 생물학적 반감기는 액체 크로마토그래피와 탠덤 질량분석기(LC-MS/MS)를 결합하여 분석한 시료 중 농약의 소실곡선으로부터 산출되었다. 분석법상의 정량한계(MLOQ)는 0.01 mg/kg 이었으며, 10 MLOQ 및 MRL (0.7 mg/kg) 두 수준에서 회수율 시험을 한 결과 각각 104.2±3.6, 101.9±10.2%의 회수율을 나타냈다. 케일 중 flubendiamide의 감소상수는 포장 1에서 0.2437, 포장 2에서 0.1981이었다. 감소상수를 사용하여 얻은 PHRL 계산식은 다음과 같이 추정되었다: 수확 10일전 잔류농도가 8.0 mg/kg 미만이라면 수확일의 잔류농도는 MRL 수준 이하일 것으로 판단된다. 세척에 의한 flubendiamide의 평균 제거율은 식초(39.8%)로 세척하였을 때 가장 높았고, 베이킹소다(31.7%), 칼슘파우더(30.2%), 중성세제(27.2%), 수돗물(15.9%) 순이었다. 본 연구의 결과는 농민과 소비자 모두에게 안전한 농산물을 생산하거나 소비하는데 유용할 것 이다.