• 제목/요약/키워드: soxhlet

검색결과 173건 처리시간 0.03초

먹는 샘물 및 PET 용기 중 Phthalate와 Adipate의 정량분석 (Quantitation of Phthalate and Adipate in Natural Mineral Water and PET Container)

  • 신원상;안혜실;신호상
    • 분석과학
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    • 제15권5호
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    • pp.475-481
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    • 2002
  • 먹는샘물과 용기 중에 phthalate 및 adipate를 분석하였다. 시료 전처리법으로서 먹는샘물의 경우는 methylene chloride를 용매로 하여 액체-액체 추출법을 사용하였고, 고체 시료는 속 슬렛 추출과 실리카겔 정제법을 사용하였다. 추출 후 농축한 다음 GC-MS (SIM)로 정량하였다. 추출물의 chromatogram은 방해물질이 없고 각 피크는 분리가 잘 되었다. 물 시료의 경우 $0.1{\sim}10{\mu}g/L$의 농도범위에서 $r^2$값이 0.996 이상의, 용기시료의 경우 $1{\sim}1,000{\mu}g/Kg$의 농도범위에서 $r^2$값이 0.994이상의 좋은 직선성을 보였다. 물 시료 중에서 검출한계는 $0.002{\sim}0.010{\mu}g/L$의 범위를 용기 시료 중에서는 $0.01{\sim}0.02{\mu}g/Kg$의 범위를 보였다. 먹는샘물 5 종류, PET병 2 종류, 라벨 2 종류, 병뚜껑 2 종류 그리고 접착제 2 종류를 위의 방법에 따라 분석하였다. 그 결과 국내산 먹는샘물 중에서는 대부분 불검출 되었고 외국산 먹는샘물에서 총 프탈레이트 $1.2{\mu}g/L$의 농도가 검출되어 외국의 경우 긴 유통기간 때문에 높은 것으로 판단되나 인체에 유해한 정도의 농도는 아니었다. 용기 재질 분석에서도 국내산 PET 용기에서 (약 0.55 mg/Kg) 보다 외국산의 경우가 (약 1.2 mg/Kg) 비교적 높은 농도로 검출되었다. 한편 라벨이나 접착제에서는 비교적 높은 농도로 프탈레이트가 함유되어 있는 것으로 나타났다. 본 연구결과 먹는샘물과 용기 중에서 프탈레이트의 분석은 공시료 분석값을 정확히 빼주는 것이 필요하며 PET 시료채취 시에는 라벨과 본드를 제외시켜야 정확한 분석값을 구할 수 있는 것으로 나타났다.

어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법 (Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography)

  • 고경목;유찬주;김종원;이석기
    • 분석과학
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    • 제31권1호
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    • pp.23-30
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    • 2018
  • 어린이 제품 중 22 종의 알러지 유발 방향성 물질들을 기체 크로마토그래피 불꽃 이온화 검출기(GC-FID)와 기체 크로마토그래피 질량 분석기(GC-MSD)를 사용하여 분석하였다. 분석물질들은 자동속슬렛 추출장치를 사용하여 추출하였으며, 고속 냉동 원심분리기에서 10분동안 원심분리 후 상징액을 2 mL vial 옮겨 Split mode로 주입하여 분석하였다. 확립된 조건에서 검정곡선은 0.996 이상의 상관계수를 갖는 직선성을 보였으며, 감도의 경우는 6.7~1,859,839로서 물질별로 기기특성 및 검출기에 따라 상당히 넓은 범위의 감도를 나타내었다. 기기검출한계는 $0.0032{\sim}0.0335{\mu}g/mL$로서 최대 약 $0.1{\mu}g/mL$이하의 기기검출한계를 나타내었고, 방법검출한계는 $0.0033{\sim}0.1161{\mu}g/mL$의 범위를 나타내었다. 또한 정량한계는 $0.0100{\sim}0.5422{\mu}g/mL$의 범위를 보였고, 정밀도는 0.21~4.89 %, 정확도는 89~111%의 범위를 나타내었다. 본 연구에서 개발한 분석법으로 시판품에 실제 적용하였다.

토양(土壤)과 채소중(菜蔬中) Phorate(0,0-diethyl S-ethylthiomethyl phosphorithioate)와 그 대사산물(代謝産物)들의 GLC분석(分析) (Determination of Phorate (0,0-diethyl S-ethylthiomethyl phosphorithioate) and its Metabolites in Soil and Vegetables by GLC)

  • 홍종욱;이해근
    • Applied Biological Chemistry
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    • 제26권2호
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    • pp.104-109
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    • 1983
  • phorate와 그 대사산물(代謝産物)들의 잔류분(殘留分) 분석방법(分析方法)을 확립(確立)코자 10% DC-200+8% Reoplex-400+2% QF-1(2 : 1 : 1, w/w/w) on Gas Chrom Q( $80{\sim}100$ mesh), $1.8m{\times}2mm$ ID, borosilicate glass column인 mixed phase column을 이용(利用), flame photometric detector가 부착(附着)된 gas chromatograph로 조사(調査)하였다. 본(本) mixed phase column은 비록 phorate와 5가지 대사산물(代謝産物)을 동시(同時)에 분리(分離)하지는 못하였으나 column온도(溫度)를 programming$(130{\sim}200^{\circ}C,\;5^{\circ}C/min)$함으로써 phoratoxon sulfoxide를 제외(除外)한 5가지 화합물(化合物)의 분리(分離)가 가능(可能)하였다(phoratoxon sulfoxide는 phoratoxon과 중첩되었음). 또는 검출감도(檢出感度)도 매우 높아 $0.05{\sim}3.15ng$범위(範圍)이었다. 한편 토양(土壤)과 채소(菜蔬)에 처리(處理)한 phorate와 그 대사산물(代謝産物)들을 methanol-acetone-benzene(1 : 1 : 1, v/v/v)으로 Soxhlet장치(裝置)에서 12시간(12時間) 추출(抽出)한 후 benzene으로 이들 화합물(化合物)을 분리(分離)한 결과(結果) 90%이상(以上)의 높은 회수율(回收率)(phoratoxon은 약(約) 84%)을 얻었다. 따라서 본(本) mixed phase column은 분리(分離)와 감도면(感度面)에서 그 성능(性能)이 우수(優秀)하여 phorate의 분해(分解)와 대사(代謝)의 연구(硏究)에 효율적(效率的)으로 이용될 수 있을 것이다.

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추출된 옥수수유와 땅콩유로부터 Conjugated Linoleic Acid를 함유한 재구성지질의 효소적 합성 및 분석 (Enzymatic Synthesis of Structured Lipids Containing Conjugated Linoleic Acid from Extracted Corn and Peanut Oil)

  • 김남숙;이기택
    • 한국식품영양과학회지
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    • 제33권6호
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    • pp.1000-1005
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    • 2004
  • 식물성 유지자원 중 옥수수와 땅콩을 원료로 하여 35$^{\circ}C$, 100 rpm의 항온교반수조와 8$0^{\circ}C$의 soxhlet extractor에서 1, 3, 6시간에 따라 유지를 추출한 후, sn-1,3 위치 특이성을 가지는 IM 60(Rhizomucor miehei, EC 3.1.1.3)를 사용하여 acidolysis 방법을 통해 CLA를 함유하는 재구성지질을 합성하였다. 추출된 옥수수유와 땅콩유 모두 35$^{\circ}C$, 6시간에서 각각 3.59, 47.98%로 여러 추출 조건 중 가장 높은 수율을 보였고, 추출된 유지 모두 phytosterol 이성질체(campesterol, stigmasterol, $\beta$-sitosterol) 중 $\beta$-sitosterol의 함량이 가장 높은 수치를 나타내었으며, oleic acid와 linoleic acid가 추출된 유지의 주요 지방산으로 조사되었다. 추출된 유지와 재구성 지질(추출유-CLA)의 tocopherol 함량 분석 결과 추출된 유지와 합성한 유지의 총 tocopherol 함량이 지정된 온도의 추출시간과 반응(합성)시간에 따라 감소되는 경향을 보였다. 한편, 재구성 지질의 지방산 조성 분석 결과 CLA 총 함량이 반응시간에 따라 증가하는 경향을 보였고 24시간 반응에서 옥수수유와 땅콩유에 결합된 CLA 총 함량이 각각 9.25, 7.48mol%로 여러 반응시간 중 가장 높게 나타났다. 또한 CLA의 주요 이성질체 중 생리활성이 높다고 알려진 cis 9, trans 11-CLA와 trans 10,cis 12-CLA의 재구성 지질 내 함량은 옥수수유와 땅콩유 각각 7.50, 6.30 ㏖%이었다.

들깨 유전자원의 지방산 변이 및 rosmarinic acid와 caffeic acid의 함량에 따른 항산화 활성 비교 (Variation in Fatty Acid Composition, Caffeic and Rosmarinic Acid Content, and Antioxidant Activity of Perilla Accessions)

  • 김다정;;정이진;전영아;이재은;이명철;이호선;이주희;성정숙
    • 한국약용작물학회지
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    • 제27권2호
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    • pp.96-107
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    • 2019
  • Background: The aim of this study was to compare the fatty acid composition, antioxidant activity, and the content of two major phenolic acids, caffeic and rosmarinic acids, of 45 Perilla accessions collected from Russia. Methods and Results: A total of 45 accessions of the genus Perilla were used in this study. The antioxidant activities of these accessions were analyzed using a spectrophotometer, and their caffeic and rosmarinic acid contents were determined using a reversed-phase ultraperformance liquid chromatography (UPLC) system. The Perilla seed oil was recovered using hexane in a soxhlet extraction method. The fatty acid compositions were analyzed using a Shimadzu QP2010 gas chromatography-mass spectoroscopy system. The results showed that accessions IT226732 and IT274300 had the highest content of caffeic and rosmarinic acid, respectively. A cluster analysis based on antioxidant assay results and concentration of phenolic acids led to the categorization of Perilla accessions into three major groups. The accessions in Group I were characterized by higher caffeic and rosmarinic acid content and antioxidant activity, compared to the accessions in the other two groups (p < 0.05). The total oil content ranged between 28.39 and 46.89%. The compositions of oleic, linoleic, and linolenic acid ranged from 11.83 to 19.55%, 11.92 to 16.71%, and 59.19 to 67.28%, respectively. Conclusions: The results of this study indicated that accessions IT274300, IT226732, IT274293, IT235818, and IT235820 could be used as a source of functional materials.

Comparison of carcass and meat quality traits between lean and fat Pekin ducks

  • Ding, Si-Ran;Li, Guang-Sheng;Chen, Si-Rui;Zhu, Feng;Hao, Jin-Ping;Yang, Fang-Xi;Hou, Zhuo-Cheng
    • Animal Bioscience
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    • 제34권7호
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    • pp.1193-1201
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    • 2021
  • Objective: According to market demand, meat duck breeding mainly includes 2 breeding directions: lean Pekin duck (LPD) and fat Pekin duck (FPD). The aim of the present study was to compare carcass and meat quality traits between 2 strains, and to provide basic data for guidelines of processing and meat quality improvement. Methods: A total of 62 female Pekin ducks (32 LPDs and 30 FPDs) were slaughtered at the age of 42 days. The live body weight and carcass traits were measured and calculated. Physical properties of breast muscle were determined by texture analyzer and muscle fibers were measured by paraffin sections. The content of inosine monophosphate (IMP), intramuscular fat (IMF) and fatty acids composition were measured by high-performance liquid chromatography, Soxhlet extraction method and automated gas chromatography respectively. Results: The results showed that the bodyweight of LPDs was higher than that of FPDs. FPDs were significantly higher than LPDs in subcutaneous fat thickness, subcutaneous fat weight, subcutaneous fat percentage, abdominal fat percentage and abdominal fat shear force (p<0.01). LPDs were significantly higher than FPDs in breast muscle thickness, breast muscle weight, breast muscle rate and breast muscle shear force (p<0.01). The muscle fiber average area and fiber diameter of LPDs were significantly higher than those of FPDs (p<0.01). The muscle fiber density of LPDs was significantly lower than that of FPDs (p<0.01). The IMF of LPDs in the breast muscle was significantly higher than that in the FPDs (p<0.01). There was no significant difference between the 2 strains in IMP content (p>0.05). The polyunsaturated fatty acid content of LPDs was significantly higher than that of FPDs (p<0.01), and FPDs had higher saturated fatty acid and monounsaturated fatty acid levels (p<0.05). Conclusion: Long-term breeding work resulted in vast differences between the two strains Pekin ducks. This study provides a reference for differences between LPD and FPD that manifest as a result of long-term selection.

Phytochemical analysis of Panax species: a review

  • Yang, Yuangui;Ju, Zhengcai;Yang, Yingbo;Zhang, Yanhai;Yang, Li;Wang, Zhengtao
    • Journal of Ginseng Research
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    • 제45권1호
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    • pp.1-21
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    • 2021
  • Panax species have gained numerous attentions because of their various biological effects on cardiovascular, kidney, reproductive diseases known for a long time. Recently, advanced analytical methods including thin layer chromatography, high-performance thin layer chromatography, gas chromatography, high-performance liquid chromatography, ultra-high performance liquid chromatography with tandem ultraviolet, diode array detector, evaporative light scattering detector, and mass detector, two-dimensional high-performance liquid chromatography, high speed counter-current chromatography, high speed centrifugal partition chromatography, micellar electrokinetic chromatography, high-performance anion-exchange chromatography, ambient ionization mass spectrometry, molecularly imprinted polymer, enzyme immunoassay, 1H-NMR, and infrared spectroscopy have been used to identify and evaluate chemical constituents in Panax species. Moreover, Soxhlet extraction, heat reflux extraction, ultrasonic extraction, solid phase extraction, microwave-assisted extraction, pressurized liquid extraction, enzyme-assisted extraction, acceleration solvent extraction, matrix solid phase dispersion extraction, and pulsed electric field are discussed. In this review, a total of 219 articles published from 1980 to 2018 are investigated. Panax species including P. notoginseng, P. quinquefolius, sand P. ginseng in the raw and processed forms from different parts, geographical origins, and growing times are studied. Furthermore, the potential biomarkers are screened through the previous articles. It is expected that the review can provide a fundamental for further studies.

Glass Dissolution Rates From MCC-1 and Flow-Through Tests

  • Jeong, Seung-Young
    • 한국방사성폐기물학회:학술대회논문집
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    • 한국방사성폐기물학회 2004년도 학술논문집
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    • pp.257-258
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    • 2004
  • The dose from radionuclides released from high-level radioactive waste (HLW) glasses as they corrode must be taken into account when assessing the performance of a disposal system. In the performance assessment (PA) calculations conducted for the proposed Yucca Mountain, Nevada, disposal system, the release of radionuclides is conservatively assumed to occur at the same rate the glass matrix dissolves. A simple model was developed to calculate the glass dissolution rate of HLW glasses in these PA calculations [1]. For the PA calculations that were conducted for Site Recommendation, it was necessary to identify ranges of parameter values that bounded the dissolution rates of the wide range of HLW glass compositions that will be disposed. The values and ranges of the model parameters for the pH and temperature dependencies were extracted from the results of SPFT, static leach tests, and Soxhlet tests available in the literature. Static leach tests were conducted with a range of glass compositions to measure values for the glass composition parameter. The glass dissolution rate depends on temperature, pH, and the compositions of the glass and solution, The dissolution rate is calculated using Eq. 1: $rate{\;}={\;}k_{o}10^{(ph){\eta})}{\cdot}e^{(-Ea/RT)}{\cdot}(1-Q/K){\;}+{\;}k_{long}$ where $k_{0},\;{\eta}$ and Eaare the parameters for glass composition, pH, $\eta$ and temperature dependence, respectively, and R is the gas constant. The term (1-Q/K) is the affinity term, where Q is the ion activity product of the solution and K is the pseudo-equilibrium constant for the glass. Values of the parameters $k_{0},\;{\eta}\;and\;E_{a}$ are the parameters for glass composition, pH, and temperature dependence, respectively, and R is the gas constant. The term (1-Q/C) is the affinity term, where Q is the ion activity product of the solution and K is the pseudo-equilibrium constant for the glass. Values of the parameters $k_0$, and Ea are determined under test conditions where the value of Q is maintained near zero, so that the value of the affinity term remains near 1. The dissolution rate under conditions in which the value of the affinity term is near 1 is referred to as the forward rate. This is the highest dissolution rate that can occur at a particular pH and temperature. The value of the parameter K is determined from experiments in which the value of the ion activity product approaches the value of K. This results in a decrease in the value of the affinity term and the dissolution rate. The highly dilute solutions required to measure the forward rate and extract values for $k_0$, $\eta$, and Ea can be maintained by conducting dynamic tests in which the test solution is removed from the reaction cell and replaced with fresh solution. In the single-pass flow-through (PFT) test method, this is done by continuously pumping the test solution through the reaction cell. Alternatively, static tests can be conducted with sufficient solution volume that the solution concentrations of dissolved glass components do not increase significantly during the test. Both the SPFT and static tests can ve conducted for a wide range of pH values and temperatures. Both static and SPFt tests have short-comings. the SPFT test requires analysis of several solutions (typically 6-10) at each of several flow rates to determine the glass dissolution rate at each pH and temperature. As will be shown, the rate measured in an SPFt test depends on the solution flow rate. The solutions in static tests will eventually become concentrated enough to affect the dissolution rate. In both the SPFt and static test methods. a compromise is required between the need to minimize the effects of dissolved components on the dissolution rate and the need to attain solution concentrations that are high enough to analyze. In the paper, we compare the results of static leach tests and SPFT tests conducted with simple 5-component glass to confirm the equivalence of SPFT tests and static tests conducted with pH buffer solutions. Tests were conducted over the range pH values that are most relevant for waste glass disssolution in a disposal system. The glass and temperature used in the tests were selected to allow direct comparison with SPFT tests conducted previously. The ability to measure parameter values with more than one test method and an understanding of how the rate measured in each test is affected by various test parameters provides added confidence to the measured values. The dissolution rate of a simple 5-component glass was measured at pH values of 6.2, 8.3, and 9.6 and $70^{\circ}C$ using static tests and single-pass flow-through (SPFT) tests. Similar rates were measured with the two methods. However, the measured rates are about 10X higher than the rates measured previously for a glass having the same composition using an SPFT test method. Differences are attributed to effects of the solution flow rate on the glass dissolution reate and how the specific surface area of crushed glass is estimated. This comparison indicates the need to standardize the SPFT test procedure.

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라이시미터를 이용한 시설하우스 내에 살포한 농약의 휘산 양상 (Volatilization of Sprayed Pesticides in Greenhouse using a Lysimeter)

  • 김단비;김택겸;권혜영;홍수명;박병준;임성진;이효섭;문병철
    • 농약과학회지
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    • 제20권4호
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    • pp.305-311
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    • 2016
  • 본 연구는 시설하우스에 살포된 농약의 공기 중 시간에 따른 분포 양상을 파악하여 농작업자의 안전성을 확보하기 위한 기초자료로 제공하기위해 수행하였다. 농작물에 많이 사용하는 물리화학적 성질이 다른 농약 10가지 성분을 선정하였으며 라이시미터 밭토양에 살포 후 공기 중으로 휘산된 양상을 720시간 동안 조사하였다. PUF 흡착제와 low volume air sampler를 이용하여 공기 중 농약을 포집한 후 LC-MS/MS를 이용하여 공기 중의 농약을 분석하였다. 720시간 동안 대부분의 농약이 24-48시간 사이에 최대 잔류를 보였다. 증기압이 1 mPa 이상의 농약은 살포 후 120-192시간까지도 공기 중 높은 농도가 지속되는 양상을 보인 반면 증기압이 1 mPa 이하인 경우에는 살포 후 첫 포집 시에 가장 높은 농도를 보이고 그 후로 계속해서 낮아지는 농도를 보였다. 공기 중의 최대 농도는 ethoprophos, diazinon, pendimethalin, chlorpyrifos, alachlor, metolachlor, carbaryl, napropamide, tebuconazole, imidacloprid 순으로 증기압의 높낮음 순서와 거의 일치하여 증기압과 휘산량의 상관관계가 높음을 알 수 있었다.

GC-tandem mass spectrometry를 이용한 분쇄원두커피 중 PAHs(polycyclic aromatic hydrocarbons) 분석법 연구 및 인체노출량 평가 (Analysis of PAHs (polycyclic aromatic hydrocarbons) in Ground Coffee Using GC-tandem Mass Spectrometry and Estimation of Daily Dose)

  • 정소영;박주성;손여준;최수정;이윤정;김미선;박소현;이상미;채영주
    • 한국식품과학회지
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    • 제43권5호
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    • pp.544-552
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    • 2011
  • 식품 중 존재하는 PAHs를 분석하기 위해 GC-MS/MS를 이용하여 분쇄원두커피를 대상으로 15종의 PAHs를 동시분석 하였다. 전처리법은 soxhlet법, 비누화분해 후 액체-액체 추출법, 초음파후 고체-액체추출법으로 비교실험하여 재현성과 불순물제거효율이 가장 좋은 초음파 후 고체-액체 추출법을 선택하여 실험하였다. 실험법의 회수율은 PAHs종에 따라 52.6-93.3%, 검출한계는 0.002-0.1 ${\mu}g/kg$, 정량한계는 0.006-0.2 ${\mu}g/kg$로 PAHs분석에 가장 좋은 감도를 나타내는 HPLC-FLD나 GC-MS-SIM과 비슷하거나 낮은 수준의 검출한계를 나타내었다. 적합한 전처리 방법을 선택한 후 시중 유통되는 원두커피를 대상으로 15종의 PAHs 함량을 조사하였을 때 46종의 총 PAHs농도는 불검출-5.988 ${\mu}g/kg$이었다. 분쇄원두커피를 커피메이커로 추출하여 PAHs의 이행계수를 계산 한 후 WHO와 U.S.EPA에서 설정한 상대독성계수(TEF)를 근거로 음용되는 원두커피의 인체노출량(mg/kg b.w./day)을 구한 결과 $5.24{\times}10^{-8}$ mg/kg b.w./day였다.