• Bulletin of the Korean Chemical Society
• /
• 제27권5호
• /
• pp.725-732
• /
• 2006

A rapid flotation methodology for zinc(II) separation and enrichment from human biofluids is established. At pH 6.0 and ambient temperature, using oleic acid (HOL) as a foaming reagent, zinc(II) was separated with phenanthraquinone monophenyl thiosemicarbazone (PPT) as a new flotation collector for Zn(II). The floated red colored 1 : 2 Zn(II)-PPT complex was measured spectrophotometrically at 526 nm with a molar absorptivity of $1.83 \;{\times}\; 10^5\; L$ mol $L ^{-1}\;cm ^{-1}$. Beer's law was obeyed over a concentration range 0.05-1.0 mg $L ^{-1}$ in the aqueous as well as in the scum layers. The proposed preconcentration flotation methodology was applied to determine Zn(II) in human biofluids. Application was, also, extended to determine Zn(II) in pharmaceutical samples and natural water samples spiked with known amounts of Zn(II) with a preconcentration factor of 100 and a detection limit of 10 ng m$L ^{-1}$. The method was verified by comparison of the spectrophotometric results with flame atomic absorption spectrometric (AAS) measurements. Moreover a postulation for the mechanism of flotation is proposed.

• 한국근적외분광분석학회:학술대회논문집
• /
• 한국근적외분광분석학회 2001년도 NIR-2001
• /
• pp.1284-1284
• /
• 2001

The transesterification of molten ethylene/vinylacetate (EVA) copolymers by octanol as a reagent and sodium methoxide as a catalyst in an extruder has been monitored by on-line near infrared (NIR) spectroscopy. A total of 60 NIR spectra were acquired for 37 minutes with the last spectrum recorded 31 minutes after the addition of octanol and catalyst was stopped. The experimental spectra show strong baseline fluctuations which are corrected for by multiplicative scatter correction (MSC). The chemometric methods of orthogonal projection approach (OPA) and multivariate curve resolution (MCR) were used to resolve the spectra and to derive concentration profiles of the species. The detailed analysis reveals the absence of completely pure variables that leads to small errors in the calculation of pure spectra. The initial estimation of a concentration that is necessary as an input parameter for MCR also presents a non-trivial task. We obtained results that were not ideal but applicable for practical concentration control. They enable a fast monitoring of the process in real-time and resolve the spectra of the EVA copolymer and the ethylene/vinyl alcohol (EVAL) copolymer to be very close to the reference spectra. The chemometric methods used and the decomposed spectra are discussed in detail.

• 한국해양학회지:바다
• /
• 제25권1호
• /
• pp.1-8
• /
• 2020

마이오세 후기(약 6.7 Ma)에 나타난 생물기원 오팔 함량의 폭감(biogenic opal crash)이 안다만해에서 획득된 IODP Site U1447과 NGHP Site 17의 코아 퇴적층에서 확인되었다. 두 코아 사이의 오팔 함량과 전반적인 변화 경향에서 나타난 차이점은 실험분석에 사용된 시약의 농도와 층서 설정에 의해 계산된 퇴적률의 차이 때문이다. 안다만해에서 발생한 마이오세 후기 생물기원 오팔 함량의 폭감은 인도네시아 관통류(Indonesian Throughflow)의 차단으로 인한 서태평양으로부터의 영양염 공급 감소와 더불어 인도여름몬순의 약화에 의한 강수량 감소로 강물에 의한 영양염 공급 감소의 복합적인 요인에 의한 것으로 제안된다.

• 한국미생물학회:학술대회논문집
• /
• 한국미생물학회 2000년도 추계학술발표대회
• /
• pp.119-127
• /
• 2000

The development and performance of a competitive indirect immunoassay for the quantitative measurement of polychlorinated biphenyl compounds in insulating oils is presented. Reagent preparation and the assay characterisation, optimisation and validation steps are described. The dynamic range of the assay for Aroclors 1254 and 1260 in methanol was $50-800 {\mu}g\;ml^{-1}$ with $50\%$ signal inhibition values of 217 and $ 212 {\mu}g\;ml^{-1}$ respectively. Impending legislation in the UK is likely to decree that oils containing $ >50 {\mu}g\;ml^{-1}$ PCB be considered contaminated. Assay sensitivity increased with the degree of PCB chlorination. The assay of structurally related compounds of environmental concern yielded cross-reactivity values of under $0.6\%$. The immunoassay proved reliable for the analysis of transformer oils containing $>70{\mu}g\;ml^{-1}$ PCB, but over-estimated PCB levels in oils containing $<20{\mu}g\;ml^{-1}$ of the analyte with the oils requiring pre-treatment using either solid-phase extraction techniques or washing with KOH-ethanol/sulphuric acid to remove matrix interferents. The analytical performance of the assay was compared against a commercially available semi-quantitative immunoassay kit for PCBs in soil and water.

• 한국해양학회지:바다
• /
• 제25권4호
• /
• pp.81-96
• /
• 2020

해수 중 용존 암모늄 분석에는 Berthlot's 반응의 분광광도법이 일반적으로 사용되었으나, 최근에는 OPA (orthophthaldialdehyde-sulfite) 형광시약을 이용한 형광법이 국제적으로 활발하게 사용되고 있다. 본 연구에서는 2017년도 호주연구선 Investigator에서 수행된 국제 영양염 선상 상호비교 실험에서 두 기관(KIOST(분광광도법, 1차 선형 회귀식 기울기만 사용), 호주CSIRO(형광법, 2차 비선형 회귀식 사용))간의 영양염 표준물질과 현장 해수시료의 용존 암모늄 농도값 차이(약 0.31 𝜇M)의 원인을 이해하기 위해 분석방법 간 검출한계, 분광광도법에 내재된 시약 굴절률, 검량선식 등에 의한 영향을 고찰하였다. 본 연구에서 측정된 분광광도법의 방법검출한계(0.063 𝜇M)와 시약 굴절률 바탕값(0.054 𝜇M)은 두 기관의 용존 암모늄 농도값 차이를 각각 20%, 17% 정도 설명할 수 있었다. 그러나 분광광도법의 검량선을 형광법과 동일한 2차식 또는 선형회기식의 기울기와 절편으로 농도를 계산할 경우, 두 기관 간의 용존 암모늄 농도값 차이는 현장에서 측정된 분광광도법의 방법검출한계 이하로 줄었다. 따라서 국제 영양염 선상 상호비교 실험에서 영양염 표준물질과 해수 현장시료에서 나타난 두 기관 간의 용존 암모늄 농도값 차이는 분광광도법과 형광법의 분석방법 차이에 의한 영향보다는 두 방법에 사용된 상이한 검량선식 영향인 것으로 판단된다. 향후 해수시료의 용존 암모늄 자료를 비교할 때 분석방법의 차이보다는 분석에 사용된 기저선, 표준용액열 개수, 검량선식 등에 대한 정보에 유의할 것을 권장한다.

• 대한임상검사과학회지
• /
• 제38권2호
• /
• pp.117-124
• /
• 2006

The analytical measurement range (AMR) is the range of analyte values that a method can directly measure on a specimen without any dilution, concentration, or other pretreatment not part of the usual assay process. The linearity of the AMR is its ability to obtain test results which are directly proportional to the concentration of analyte in the sample from the upper and lower limit of the AMR. The AMR validation is the process of confirming that the assay system will correctly recover the concentration or activity of the analyte over the AMR. The test specimen must have analyte values which, at a minimum, are near the low, midpoint, and high values of the AMR. The AMR must be revalidated at least every six months, at changes in major system components, and when a complete change in reagents for a procesure is introduced; unless the laboratory can demonstrate that changing the reagent lot number does not affect the range used to report patient test results. The AMR linearity was total protein (0-16.6), albumin (0-8.1), total bilirubin (0-18.1), alkaline phosphatase (0-1244.3), aspartate aminotransferase (0-1527.9), alanine aminotransferase (0-1107.9), gamma glutamyl transpeptidase (0-1527.7), creatine kinase (0-1666.6), lactate dehydrogenase (0-1342), high density lipoprotein cholesterol (0.3-154.3), sodium (35.4-309), creatinine (0-19.2), blood urea nitrogen (0.5-206.2), uric acid (0-23.9), total cholesterol (-0.3-510), triglycerides (0.7-539.6), glucose (0-672.7), amylase (0-1595.3), calcium (0-23.9), inorganic phosphorus (0.03-17.0), potassium (0.1-116.5), chloride (3.3-278.7). We are sure that materials for the AMR affect the evaluation of the upper limit of the AMR in the process system.

• 분석과학
• /
• 제19권1호
• /
• pp.107-114
• /
• 2006

본 연구에서는 trimethylsilyl (TMS) 및 trifluoroacetyl (TFA)유도체화를 이용하여 소변여지에서 대사이상 질환을 신속하게 스크리닝하는 GC/MS 분석법을 개발하였다. 유기산과 아미노산을 동시에 유도체화하기 위해 메틸오렌지를 지시약으로 하여 $60^{\circ}C-70^{\circ}C$에서 15-20 분간 카르복실기는 TMS로 아미노기는 TFA로 유도체한 후 GC/MS-SIM으로 분석하였다. 유기산과 아미노산의 직선성의 범위는 0.001-50 mg이었고, 소변에서의 검출한계는 10-200 ng, 정량한계는 80-900 ng 이었다. 직선성을 보이는 범위에서의 상관계수(R2)는 0.994-0.998이었고, 회수율은 methylcitric acid와 glycine을 제외하고 80-100%를 보였다. 이 방법은 기존의 유기산분석에는 GC/MS를 아미노산 분석에는 아미노산분석기를 사용하는 것과 비교할 때 GC/MS만 사용하여 동시에 유기산과 아미노산을 분석함으로써 전처리가 간단하고 짧은 분석시간과 우수한 감도, 정확도, 정밀도를 보여 주었다. 정상인과 대사이상질환 환자의 검체에 적용해 보았을 때, 본 분석방법은 유기산과 아미노산대사이상의 유전성대사질환 환자의 스크리닝, 진단 및 모니터링에 임상적으로 유용함을 보여주었다.

• 한국토양비료학회지
• /
• 제31권2호
• /
• pp.114-119
• /
• 1998

토양(土壤)의 인산분석(燐酸分析)의 정확도(正確度)를 향상(向上)시킬 수 있는 인산 발색방법을 찾고자 인산농도(燐酸濃度)가 다른 Lancaster, Mehlich II, Mehlich III 추출액(抽出液) 그리고 증류수중(蒸溜水中)의 인산을 Amino - Naphtol -Sulfonic acid(ANS), Ascorbic acid (AA)-Antimony potassium tartarate 그리고 Ascorbic acid-Bismuth subcarbonate(AB) 법(法)등 3개(個) 발색정양법(發色定量法)으로 발색 정치시간(靜置時間)을 달리하면서 Hitachi U-2000 분광분석기(分光分析器)로 분석(分析)한 결과(結果)는 다음과 같다. 인산 발색정치시간을 0.5시간으로 고정하여 분석된 표준액의 인산값과 여러수준의 시간을 두고 분석된 각 시료용액의 인산값간의 상관관계에서 ANS방법을 사용한 경우 발색을 위한 정치시간이 경과 할 수록 색도가 높아져 1차회귀계수가 커졌으나 Ascorbic acid를 사용한 AA와 AB법은 3시간의 발색에서도 흡광도의 안정성을 보였고, 분석치의 변이계수도 ANS법보다 낮았다. 인의 검량범위는 ANS법이 가장 넓으나 저농도에서는 분석의 정확도가 낮고 AA와 AB법은 저농도에서도 정확도가 높았으며 AB법은 AA법보다 넓은 범위의 인 농도 측정이 가능하였다. 따라서 3종의 인산발색법중 수용성 인 분석에는 AA법이 가장 좋았고 시약으로 추출되는 인 분석에는 AB법이 우수한 것으로 판단되었다.

• 대한약침학회지
• /
• 제15권4호
• /
• pp.42-51
• /
• 2012

Objectives: This study used the basic principle of Oriental medicine, the sovereign, minister, assistant and courier principle (君臣佐使論) to investigate the effects of the component of ONGABO, which is composed of Ginseng Radix (Red Ginseng), Angelica Gigantis Radix, Schisandrae Fructus, Cuscuta Semen and Curcumae tuber on the viability of HepG2 cells. Methods: Single and mixed extracts of the component of ONGABO were prepared by lypohilizing powder of Red Ginseng (6-year root from Kanghwa), Angelica Gigantis Radix, Schisandrae Fructus, Cuscuta Semen, Curcumae Tuber (from Omniherb Co., Ltd., Korea) at the laboratory of herbal medicine in Woosuk University and were eluted after being macerated with 100% ethanol for three days. The cell viability of HepG2 was determined by using an absorptiometric analysis with PrestoBlue (Invitrogen) reagent after the plate had been incubated for 48 hours. All of the experiments were repeated three times to obtain the average value and standard deviation. The statistical analysis was done and the correlation factor was obtained by using Microsoft Office Excel 2007 and Origin 6.0 software. Results: Although Ginseng Radix (Red Ginseng) and Schisandrae Fructus did not enhance the viability of HepG2 cells, they were shown to provide protection of those cells. On the other hand, Angelica Gigantis Radix decreased the viability of HepG2 cells significantly, Cuscuta Semen and Curcumae Tuber had a small or no effect on the viability of HepG2 cells. Conclusions: In the sovereign, minister, assistant and courier principle (君臣佐使論), Ginseng Radix (Red Ginseng) corresponds to the sovereign component because it provides cell protection effects, Angelica Gigantis Radix corresponds to minister medicinal because it kills cells, Schisandrae Fructus corresponds to the assistant medicinal to help red ginseng having cell protect effects. Cuscuta Semen and Curcumae Tuber correspond to the courier medicinal having no effect in cell viability in HepG2. We hope this study provides motivation for advanced research on the sovereign, minister, assistant and courier principle.

• Bulletin of the Korean Chemical Society
• /
• 제35권11호
• /
• pp.3275-3279
• /
• 2014

A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.