• 제목/요약/키워드: HPLC- MSD

검색결과 44건 처리시간 0.022초

대기 중 휘발성유기화합물질 및 알데하이드의 분석 신뢰도 향상에 관한 고찰 (Study on Improvement in Reliability of Analysis for VOCs and Aldehydes)

  • 이민도;이상욱;임용재;김영미;김소영;문광주;한진석;정일록
    • 한국대기환경학회지
    • /
    • 제22권4호
    • /
    • pp.468-476
    • /
    • 2006
  • Hazardous air pollutants (HAPs) have high toxicity and bioaccurnulation potentials into human body even inbsmall amount (levels of ng/$m^3$). As the levels of HAPs might be controversial, it has been become essential to establish the analysis method for correct results. In this study, various analysis methods of VOCs and Aldehydes were compared in order to select the proper methods in our condition. Sampling and analysis method of VOCs were followed to EPA TO-14a and TO-17. VOCs were collected in absorption tube and separated by thermal desorption unit then analyzed by GC/MSD. Aldehydes were sampled in DNPH-cartridge and extracted into solution then analyzed by HPLC as the same condition of EPA TO-13a. This study also shows the results of QA/QC system of selected methods. Some experiments could be improving the data assurance blank test, calibration check, repetition precision check, the determination of detection limit and reproducibility of the retention time. Precisions of VOCs and aldehydes were ranged in 2$\sim$9% and 1$\sim$4% RSD, respectively. Recovery rate of VOCs showed variable ranges from 60 to 133.5%. MDL of VOCs and aldehydes were 0.044$\sim$0.284 ppb and 0.14$\sim$1.02 ng, respectively.

Monitoring and Risk Assessment of Pesticide Residues in Commercially Dried Vegetables

  • Seo, Young-Ho;Cho, Tae-Hee;Hong, Chae-Kyu;Kim, Mi-Sun;Cho, Sung-Ja;Park, Won-Hee;Hwang, In-Sook;Kim, Moo-Sang
    • Preventive Nutrition and Food Science
    • /
    • 제18권2호
    • /
    • pp.145-149
    • /
    • 2013
  • We tested for residual pesticide levels in dried vegetables in Seoul, Korea. A total of 100 samples of 13 different types of agricultural products were analyzed by a gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography- ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze for 253 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 11 samples, of which 2 samples (2.0%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in 6 of 9 analyzed dried pepper leaves and 1 sample exceeded the Korea MRLs. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The estimated daily intakes (EDIs) range from 0.1% of the acceptable daily intake (ADI) for bifenthrin to 8.4% of the ADI for cadusafos. The most critical commodity is cadusafos in chwinamul, contributing 8.4% to the hazard index (HI). This results show that the detected pesticides could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring is recommended.

독활(獨活)과 그 위품의 감별기준 연구 : 외·내부형태 및 이화학패턴을 중심으로 (A Study on Identification Keys of Araliae Continentalis Radix and its Adulterants : Focused on External·Internal Morphology and Pattern Analysis)

  • 윤지현;주영승
    • 대한본초학회지
    • /
    • 제33권2호
    • /
    • pp.29-43
    • /
    • 2018
  • Objectives : Araliae Continentalis Radix(AC) is a medicinal herb belonging to the drug efficacy group treating musculoskeletal disorders(MSD) with anti-inflammatory, analgesic and antipyretic action. However, due to morphologic and onomastic similarity, adulterants(Angelicae Pubescentis Radix: AP, Gypsophilae Oldhamianae Radix: GO, Levistici Officinalis Radix: LO) have been included or replaced the standard. Methods : Multilateral methods were carried out on the identification of AC and its adulterants. Macroscopic and microscopic characteristics were observed by using stereoscope and microscope. For the comparison of chromatogram pattern, standard compounds were analyzed simultaneously using high performance liquid chromatography. Results : 1. The macroscopic identification of original plants was determined by the phyllotaxis type, the inflorescence type, the leaf margin and the color of flowers. The macroscopic identification of herbal materials was examined by oil spots, the cambium, heteromorphic vascular bundles, and the pholem. 2. For the microscopic identification, the fact whether its xylem ray is proliferated or not was first determined. Then medicinal herbs were secondly divided by cellular inclusions, fiber bundles, the distribution of secretary canals and the shape of cambium. 3. AC and its adulterants showed different chromatographic fingerprints. AC was containing continentalic acid and kaurenoic acid. AP was containing osthole and columbianadin. LO was containing osthole and falcarindiol. None of the compounds were found in GO. Conclusions : This recent identification keys of might be helpful to discriminate the pharmacopoeia standard and its adulterants for the right usage in clinics.

Identification and Characterization of Phytochemicals from Peanut (Arachis hypogaea L.) Pods

  • Lee, Jin-Hwan;Baek, In-Youl;Ha, Tae-Joung;Choung, Myoung-Gun;Ko, Jong-Min;Oh, Sea-Kwan;Kim, Hyun-Tae;Ryu, Hyung-Won;Park, Keum-Yong;Park, Ki-Hun
    • Food Science and Biotechnology
    • /
    • 제17권3호
    • /
    • pp.475-482
    • /
    • 2008
  • Methanol extracts of peanut (Arachis hypogaea L.) pods were chromatographed, which yielded 3 phytochemicals 1-3 including 5,7-dihydroxychromone (1), eriodictyol (2), and 3',4',5,7-tetrahydroxyflavone (3). To confirm the presence of isolated phytochemicals, the pods extracts were performed by high performance liquid chromatography coupled with a photodiode array detector (HPLC-PDA) and a mass spectrometric detector (MSD) with electrospray ionization (ESI). Optimum extraction conditions for phytochemical contents using peanut germplasm were obtained by employing 90% MeOH for 12 hr at room temperature and phytochemicals 1-3 showed significant differences with concentrations of $407.56{\pm}23.35$, $52.92{\pm}5.11$, and $2,024.34{\pm}134.18\;{\mu}g/g$, respectively. Under this optimal conditions, the contents of phytochemicals 1-3 in peanut pods of 3 Korea cultivars including 'Jakwang', 'Daekwang', and 'Palkwang' exhibited phytochemical 3 was the highest range of $1,338.01-5,162.93\;{\mu}g/g$, followed by phytochemical 1 ($590.13-1,382.10\;{\mu}g/g$), and phytochemical 2 ($25.12-186.85\;{\mu}g/g$), respectively. Moreover, 'Jakwang' exhibited the highest contents of phytochemical (1: $1,362.10{\pm}52.49$, 2: $186.85{\pm}17.69$, and 3: $5,162.93{\pm}148.64\;{\mu}g/g$, respectively), whereas the lowest contents was found in the 'Daekwang' (1: $590.13{\pm}22.23$, 2: $25.12{\pm}2.45$, and 3: $1,338.01{\pm}62.17\;{\mu}g/g$, respectively). These results suggest that the methanol extracts of peanut pods may possess health related benefits to humans owing to various known biological activities of phytochemicals 1-3.

유통 친환경 엽채류와 엽경채류 중 잔류농약 실태조사 및 안전성 평가 (Monitoring of Pesticide Residues in Commercial Environment-friendly Stalk and Stem Vegetables and Leafy Vegetables and Risk Assessment)

  • 이재윤;노현호;이광헌;박소현;경기성
    • 농약과학회지
    • /
    • 제16권1호
    • /
    • pp.43-53
    • /
    • 2012
  • 국내 유통 친환경인증 엽채류와 엽경채류 중 잔류농약 실태를 파악하기 위해 서울 등 전국 9개 지역의 대형마트와 친환경인증 농산물 판매소에서 상추 등 21종의 친환경인증 엽채류 및 엽경채류를 2010년 7월과 8월 2회 채취 하였으며, 총 시료수는 637(유기농산물 395, 무농약농산물 242)점이었다. 수집된 시료는 GC-ECD/NPD, HPLC-DAD/FLD를 이용한 다성분 동시분석법으로 잔류농약을 분석하였다. 분석 결과 양배추 등 8점의 시료에서 alachlor를 포함한 6종의 농약이 검출되어 1.3%의 검출율을 보였으며, 검출농약의 잔류량은 alachlor 0.043, chlorfenapyr 0.022-0.324, diazinon 0.024, dicofol 0.05-0.138, dithiopyr 0.008, metolachlor 0.025 mg/kg이었다. 시료에서 검출된 농약의 잔류량은 모두 잔류허용기준을 초과하지 않았고 일일섭취추정량 대비 일일섭취허용량은 25% 미만으로 안전한 것으로 판단되었으나 농약이 검출된 시료 중 5점은 친환경농산물 인증기준을 초과하여 부적합 농산물로 분류되었다.

포사맥스 정(알렌드론산나트륨 70 mg)에 대한 대웅 알렌드로네이트 정 70 mg의 생물학적동등성 (Bioequivalence of Daewoong AlendronateTM Tablet to FosamaxTM Tablet (Sodium Alendronate 70 mg))

  • 이예리;정선경;양승권;최기호;신용철;전형규;강승우;이희주
    • Journal of Pharmaceutical Investigation
    • /
    • 제36권2호
    • /
    • pp.137-142
    • /
    • 2006
  • A bioequivalence of Daewoong $Alendronate^{TM}$ (Daewoong Pharmaceutical Co., Ltd., Korea) and $Fosamax^{TM}$ tablets (MSD Korea) was evaluated according to the guideline of Korea Food and Drug Administration (KFDA). A single 70 mg dose of sodium alendronate of each medicine was administered orally to 56 healthy male volunteers. This study was performed in a $2\;{\time}\;2$ crossover design. Concentrations of alendronate in the urine were monitored by a high-performance liquid chromatography (HPLC). $A_{et}$ (cumulative urinary excreted amount from time 0 to last sampling interval) was calculated by the accumulation of the urinary excreted alendronate. $U_{max}$ (maximum urinary excretion rate) and $T_{max}$ (time to reach $U_{max}$) were compiled from the urinary excretion rate - time data. Analysis of variance was performed using logarithmically transformed $A_{et}$ and $U_{max}$. No significant sequence effect was found for all of the bioavailability parameters. The 90% confidence intervals of the $A_{et}$ and $U_{max}$ for Daewoong $Alendronate^{TM}/Fosamax^{TM}$ were 0.89-1.12 and 0.82-1.02, respectively. This study demonstrated the bioequivalence of Daewoong $Alendronate^{TM}$ and $Fosamax^{TM}$ with respect to the rate and extent of absorption.

프로스카 정(피나스테리드 5 mg)에 대한 푸로케어 정의 생물학적동등성 (Bioequivalence of Procare Tablet to Proscar® Tablet (Finasteride 5 mg))

  • 강현아;조혜영;이용복
    • Journal of Pharmaceutical Investigation
    • /
    • 제36권2호
    • /
    • pp.143-148
    • /
    • 2006
  • Finasteride $[N-(1, 1-dimethylethyl)-3-oxo-4-aza-5{\alpha}-androst-1-ene-17{\beta}-carboxamide]$ is a 4-aza-3-oxosteroidal inhibitor of human $5{\alpha}-reductase$. The purpose of the present study was to evaluate the bioequivalence of two finasteride tablets, $Proscar^{\circledR}$ (MSD Korea Ltd.) and Procare (Hana Pharm. Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The release of finasteride from the two finasteride formulations in vitro was tested using KP VIII Apparatus II method with various dissolution media (pH 1.2, 4.0, 6.8 buffer solution and water). Twenty six healthy male subjects, $23.7\;{\pm}\;2.24$ years in age and $67.2\;{\pm}\;8.55\;kg$ in body weight, were divided into two groups and a randomized $2\;{\time}\;2$ cross-over study was employed. After two tablets containing 5 mg as finasteride was orally administered, blood samples were taken at predetermined time intervals and the concentrations of finasteride in serum were determined using HPLC with UV detector. The dissolution profiles of two formulations were similar in all tested dissolution media. The pharmacokinetic parameters such as $AUC_t,\;C_{max},\;and\;T_{max}$ were calculated and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t,\;C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug, $Proscar^{\circledR}$, were 6.39, 4.65 and -13.9% for $AUC_t,\;C_{max},\;and\;T_{max},$ respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.800 to log 1.25 $(e.g.,\;log\;0.990{\sim}log\;1.14\;and\;log\;0.977{\sim}log\;1.13 for\;AUC_t\;and\;C_{max},\;respectively)$. Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating Procare tablet was bioequivalent to $Proscar^{\circledR}$ tablet.

열처리 양파로부터 항산화물질의 분리동정 (Isolation and Identification of an Antioxidant Substance from Heated Onion (Allium cepa L.))

  • 황인국;김현영;이상훈;황초롱;오승희;우관식;김대중;이준수;정헌상
    • 한국식품영양과학회지
    • /
    • 제40권3호
    • /
    • pp.470-474
    • /
    • 2011
  • 열처리한 양파 착즙액의 ethyl acetate 분획물로부터 항산화물질을 분리 동정하기 위하여 1, 2차 silica gel column chromatography, preparative TLC 및 HPLC를 이용하여 항산화활성 물질을 분리 정제하였다. GC/MSD, $^1H$-NMR 및 $^{13}C$-NMR spectrum 결과로부터 구조 동정한 결과 분리된 물질은 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one(DDMP)으로 확인되었다. DDMP의 항산화활성의 $IC_{50}$값은 241.6 ${\mu}g/mL$이었으며, vitamin E의 69.2 ${\mu}g/mL$와 C의 45.3 ${\mu}g/mL$보다는 낮은 활성을 보였고 BHT의 268.0 ${\mu}g/mL$보다는 높은 활성을 보였지만 유의적인(p>0.05) 차이는 나타나지 않았다. 추후 DDMP를 기능성물질로 활용하기 위하여 다양한 생리활성 평가가 필요할 것으로 생각된다.

서울지역 유통 채소류의 잔류농약 조사 (The Survey on Pesticide Residues in Vegetables Collected In Seoul)

  • 장미라;문현경;김태랑;육동현;김은희;홍채규;최채만;황인숙;김정헌;김무상
    • 농약과학회지
    • /
    • 제15권2호
    • /
    • pp.114-124
    • /
    • 2011
  • 본 연구는 2007년부터 2009년까지 서울지역에서 유통 중인 채소류 91종 18,069건에 대해 GC와 HPLC 및 GC-MSD를 이용한 다성분 동시분석법으로 잔류 농약을 분석하여 농약의 잔류실태를 파악하였다. 채소류 중 잔류농약 검출비율은 2007년 11.2%, 2008년 8.5%, 2009년 12.0%로 나타났으며, 잔류허용기준초과비율은 2007년 4.6%, 2008년 2.8%, 2009년 2.1%로 감소하는 경향을 나타내었다. 농약 잔류허용기준을 초과한 농약성분은 각각 2007년 43종, 2008년 30종, 2009년 36종이었으며, 이 중 2007년에는 azoxystrobin이 71회, 2008년에는 procymidone이 29회, 2009년에는 endosulfan이 24회로 가장 많았다. 3년 동안 연도별로 10건 이상 분석한 채소류의 시료수 대비 농약 잔류허용기준 초과비율은 겨자채가 가장 높게 나타났다. 검출빈도가 높은 농약성분에 대해 연도별 농약 잔류량을 비교한 결과 diazinon, endosulfan, paclobutrazol, procymidone 검출량이 통계적으로 유의한 차이가 있는 것으로 나타났다.

동시 다성분 분석법에 의한 농산물 중 Diflubenzuron 분석 (Analysis of Diflubenzuron in Agricultural Commodities by Multiresidue Method)

  • 박선희;한창호;김애경;신재민;이재규;박영혜;김지민;황래홍;장민수;송미옥;박주성;윤은선;김무상;정권
    • 농약과학회지
    • /
    • 제18권4호
    • /
    • pp.269-277
    • /
    • 2014
  • HPLC-UVD를 이용하여 diflubenzuron이 다종농약다성분 분석법 제2법에 적합한지를 검증하고자 본 연구를 수행하였다. 유효성을 검증하기 위하여 농약이 검출되지 않은 시금치, 엇갈이배추, 가지, 애호박, 청피망, 오이, 참외 등 7종 농산물을 대상으로 직선성, 특이성, 검출한계, 정량한계, 정확성, 정밀성을 확인하였다. Diflubenzuron 표준용액을 0.05-5 mg/kg 농도로 희석하여 분석한 표준검량선의 직선성은($R^2=0.99999$)은 매우 만족할 만한 수준이었다. 검출한계는 0.008 mg/kg, 정량한계는 0.02 mg/kg 이며 회수율은 77.5-105.6%, 상대표준편차는 최대 20% 미만, 정밀도는 intra-day test에서 0.4-1.9%, inter-day test에서 0.7-1.9%를 나타내어 잔류농약분석법에서 허용하는 회수율 기준 70-120% 범위와 상대표준편차 20% 이하의 기준에 적합하였다. LC-MSD를 이용한 재확인 과정을 통해 잔류결과의 신뢰성을 확보하였다. 따라서 유통농산물 중 diflubenzuron의 일상적 검사법으로 빠르고 간편한 다종농약다성분 제2법을 적용할 수 있을 것으로 판단된다.