• Bulletin of the Korean Chemical Society
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• 제15권11호
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• pp.945-949
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• 1994

Mixtures of cyano complexes of palladium(II) and platinum(II) were separated by capillary electrophoresis using a fused silica capillary as a separation column and 30 mM phosphate buffer (pH 7) containing 15 wt. % acetonitrile as a running buffer. By virtue of the high ionic mobilities of the negatively charged cyano complexes of Pd(II) and Pt(II), they were separated using a cathodic injection and anodic detection scheme. The metal complexes eluted through the capillary were detected by direct UV absorption at 214 nm. A linear relationship between peak area and concentration was obtained for both ions and the detection limit was lower than $10^{-14}$ mole. The proposed method was applied to real sample, e.g., anode slime obtained from an electrolytic copper refinary, as a method for the simultaneous determination of palladium and platinum.

• Mass Spectrometry Letters
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• 제14권3호
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• pp.104-109
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• 2023

Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

• Journal of the Optical Society of Korea
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• 제20권6호
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• pp.669-677
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• 2016

A miniaturized FTIR spectrometer based on lamellar grating interferometry is being developed for passive remote-sensing. Consisting of a pair of micro-mirror arrays, the lamellar grating can be fabricated using MEMS technology. This paper describes a method to compute the optical field in the interferometer to optimize the design parameters of the lamellar grating FTIR spectrometer. The lower limit of the micro-mirror width in the grating is related to the formation of a Talbot image in the near field and is estimated to be about $100{\mu}m$ for the spectrometer to be used for the wavelength range of $7-14{\mu}m$. In calculating the far field at the detection window, the conventional Fraunhofer equation is inadequate for detection distance of our application, misleading the upper limit of the micro-mirror width to avoid interference from higher order diffractions. Instead, the far field is described by the unperturbed plane-wave combined with the boundary diffraction wave. As a result, the interference from the higher order diffractions turns out to be negligible as the micro-mirror width increases. Therefore, the upper limit of the micro-mirror width does not need to be set. Under this scheme, the interferometer patterns and their FT spectra are successfully generated.

• 한국수산과학회지
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• 제56권4호
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• pp.428-437
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• 2023

A simultaneous analytical method was developed and validated for the analysis of prohibited fluoroquinolone (FQ) antibiotics including norfloxacin, ofloxacin, and pefloxacin, released by aquaculture in seawater and effluents. The samples were filtered, and extracts were obtained using a solid phase extraction cartridge with methanol (MeOH). The extracts were concentrated, and analyzed using ultra-performance liquid chromatography-tandem mass spectrometry. Two different columns and four different mobile phases were compared to achieve optimal separation and sensitivity for target compounds. Typical validation parameters including linearity, recovery of surrogate standard, instrument detection limit (IDL), limit of quantification (LOQ), and method detection limit (MDL) were evaluated. The linearity of calibration curves was over 0.999. Recoveries of surrogate ranged from 87.6% to 113%. The LOQ of target compounds was approximately 3-8 times lower than those reported in previous studies. The IDL and MDL were 0.06-0.57 and 0.06-0.37 ng/L, respectively. Seven effluent samples collected from an aquaculture located in Jeju were analyzed; however, not all target compounds were detected in the samples, suggesting that the banned antibiotics were not used. Overall, this established method was able to simultaneously analyze the three FQ antibiotics, and may be useful for monitoring prohibited antibiotics in the fishery industry.

• 농약과학회지
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• 제16권2호
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• pp.85-97
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• 2012

2006년부터 2010년까지 경기도내에서 유통되는 과실류 33품목에 대하여 잔류농약 모니터링을 수행하였다. 총 2,558건 중 431건(16.8%)에서 잔류농약이 검출되었으며, 12건(0.5%)에서 잔류허용기준(MRLs)을 초과하였다. 연간 검출률은 6.9~19.4%, 부적합률은 0.3~0.9%였다. 23품목에서 62종의 잔류농약이 검출되었고, 4품목에서 8종의 농약이 부적합 발생하였다. Chlorpyrifos의 검출빈도가 가장 높았다. 과실류 중 감귤류가 검출률과 부적합률 모두 가장 높았다. 검출빈도는 유기인계 농약이(35%) 가장 많았고, 용도별로는 살충제가(57%) 가장 많았다. 결정론적 만성식이위해평가 결과 위해도(%ADI)는 전국민 하한치와 상한치가 각각 0.0000~0.7526과 0.0000~1.3237이었고, 섭취자군에서는 각각 0.0006~9.7801과 0.0058~15.9528로 나타나 전국민과 섭취자군 모두에서 안전한 수준으로 나타났다.

• KSBB Journal
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• 제13권5호
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• pp.577-584
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• 1998

A sensitive membrane strip assay for plasma lipoprotein cholesterol that can be performed without handling reagents has been investigated. We previously developed an assay system with immobilized enzymes (cholesterol esterase and cholesterol oxidase) on the surfaces of nitrocellulose membrane(1). In such a case, the amount of enzymes present on the membrane was limited by its surface area and, thus, the detection capability was relatively poor (> 50 mg/dL cholesterol). To overcome this problem, we devised a new system with non-immobilized enzymes by placing them within interstitial spaces of a celullose membrane pad in a dry state. Upon contact with sample medium, the enzymes were immediately dissolved and participated in the reactions with cholesterol in a liquid phase. We constructed a user-friendly system consisting of four membrane pads fro sample application, cholesterol decomposition, color development as signal, and medium absorption to invoke a continuous flow (sequential location from the bottom). A sample containing lipoproteins was added into the application pad by capillary action and transferred to the next pad for decomposition. The decomposition pad (namely, enzyme pad) contained a detergent (sodium cholate) for the destruction of lipoprotein particles, the two enzymes for cholesterol decomposition, and a chromogen (3,3'-diaminobenzidine). As a consequence of the enzyme reactions, hydrogen peroxide was produced, and then reacted in the presence of the chromogen with horseradish peroxidase immobilized on the signal generation pad. Finally, a colorimetric signal directly proportional to the cholesterol concentration was produced. The detection limit determined from this system under optimal conditions was at least 2 times lower than of the enzyme-immobilized system.

• Journal of Periodontal and Implant Science
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• 제26권1호
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• pp.161-175
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• 1996

There were many reports that elevations in the levels of active and latent collagenase in gingival crevicular fluid(GCF) have been correlated positively with periodontal disease activity. To provide a simple diagnostic approach for testing GCF collagenolytic activity, the detection limit of enzyme activity was compared using radiofibril assay(Sodek et.al.1981) and spectrophotometric collagenolytic assay(Nethery et al. 1986). The detection limits of both assay for standard bacterial enzyme were similar and the radiofibril assay showed a little (1/2) lower detection limit for tad pole collagenase. To evaluate the relationship between periodontal tissue destruction and the collagenolytic activity, GCF was collected, and latent and active enzyme activities were measured by a spectrophotometric collagenolytic assay. Twelve subjects showing progressive lesions were selected according to the presence of immediate tissue destruction, frequent abscess formation, and increasing need for tooth extraction, and the absence of underlying systemic disease and previous antibiotic medication history within 6 months. Comparisons were made between sites with either: 1) inflammation with a previous history of progressive loss of periodontal tissue and bone support(2l progressive sites): 2) previous history of bone loss and periodontal destruction but now clinically stable(12 comparably stable sites); or 3) no loss of periodontal tissue and bone support(11 control sites including 5 gingivitis sites and 6 healthy sites). Active collagenase activity was the highest in the progressive sites and decreased in the order of the gingivitis sites, the stable sites, and the healthy sites. The total enzyme activity was $2{\sim}3$ fold higher in the progressive sites and the gingivitis sites, compared to the stable and the healthy sites. The ratio of active to total collagenolytic activity was twice in the progressive sites. Analysis of active collagenase level(5mU) and the ratio of active to total collagenolytic activity(0.8) as a diagnositic test indicates that these measurements have the sensitivity of 0.81 and 0.86, the specificity of 0.70 and 0.65, and the overall agreement of 0.75 and 0.73, respectively. Thus, this method has significant merits as a diagnostic tool to determine wherher the site is in a state of remission or progression.

• Toxicological Research
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• 제26권2호
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• pp.149-155
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• 2010

The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with ${\mu}$-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and $11.1{\mu}g/l$, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to $250{\mu}g/l$. The intra- and inter-day accuracy (n = 6) ranged from 89.2% to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples.

• 암석학회지
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• 제10권3호
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• pp.179-189
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• 2001

전자현미분석 기를 이용한 저어콘 및 모나자이트의 화학적 연대측정은 미량의 U, Th 및 Pb의 정량분석을 통해 이루어지는데, 측정에 이용되는 M-line의 특성 X-선은 발생효율이 낮고 피크강도가 작아 측정하한과 오차범위가 고려된 분석조건이 설정 되어야한다. 총 분석시간을 줄이고, 측정조건의 변위에 따른 오차를 감소시키고자 PET결정을 갖춘 3개의 분광기를 이용하여 U, Th 및 Pb를 동시에 측정하였고, 파고분석기를 이용하여 피크/배경 비율을 증가시켜 측정하한을 낮추었다 최적 분석조건하에서 U, Th 및 Pb에 대한 이론적 값인 측정하한을 30 ppm (99%유의수준)까지 낮출 수 있었고. 저어콘의 단일측정 시 800 ppd의 Pb농도에서 $\pm$10% ($2{\sigma}$), 2330 ppm의 U에서 $\pm$5% ($2{\sigma}$) 그리고 측정된 연대에서 $\pm$10% ($2{\sigma}$)이내의 상대오차범위에서 분석결과를 얻었다. 저어콘 및 모나자이트의 연대측정을 수행하는데 있어, 3 $\mu\textrm{m}$ 이하의 공간분해능, 100 ppm ($3{\sigma}$) 이하의 측정하한과 $\pm$10% ($2{\sigma}$) 이하의 분석오차를 고려한 가속전압은 15~20 keV, 빔 전류는 100~200 nA, 그리고 총 측정시간을 300~l200초 (피크와 배경위치에서 각각 동일한 시간으로 측정)로 설정하여 보다 정밀하고 정확한 분석자료를 얻을 수 있었다. 높은 전류에 따른 시료의 손상을 줄이기 위해선 전자빔 직경을 3~5 $\mu\textrm{m}$로 증가시키거나 보다 짧은 시간동안의 측정을 반복하여 그 평균값을 이용하는 것이 필요하다. 빔 전류를 증가시키거나 분석시간을 늘려 측정하한을 낮추고 정밀도를 향상시킴으로서 보다 젊은 시기의 암석이나 상대적으로 U, Th 및 Pb의 함량이 적은 광물의 연대측정에 이용할 수 있다.

• 대한임상검사과학회지
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• 제36권2호
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• pp.127-130
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• 2004

Analytical sensitivity on TDM test is the lowest concentration that can be distinguished from background noise. The aim of study was to evaluate analytical sensitivity that is also referred to as the lower limit of detection(LLD) about difference between zero calibrator and isotonic saline sample. We tested for 10 days with zero calibrators and 0.85% saline samples while running trilevel control samples under control. Raw data divided by two groups calculated mean and standard deviation from two sample populations and analytical sensitivity by ${\bar{X}}+2SD$. In comparison with isotonic saline samples and zero calibrators, there were significant differences in phenytoin, phenobarbital and vancomycin, etc. Especially analytical sensitivity on phenytoin is at the same level as the upper limit of analytical measurement range with $40{\mu}g/mL$. We think the cause of this is matrix interference. In conclusion, we were sure that standard protocol for analytical sensitivity as lower limit of analytical measurement range on TDM test must be measured with zero standard rather than an isotonic saline sample and type 1 reagent DW for reducing matrix effects within interactions between different materials in a mixture.