• 분석과학
• /
• 제15권5호
• /
• pp.410-416
• /
• 2002

본 연구에서는 LC - MS/MS를 이용해 혈장과 뇨중에서 반코마이신을 신속하게 정량분석하는 방법을 개발하였다. 크로마토그래피는 $C_{18}$ XTerra MS 컬럼 ($2.1{\times}30mm$, $3.5{\mu}m$)을 사용하여 분석하였다. 이동상으로는 0.25% 초산이 섞인 10% 아세토니트릴 용액을 사용하였으며, 유속은 $250{\mu}L/min$이다. 반코마이신과 카페인 (내부표준물질)은 multiple reaction monitoring (MRM) 방법을 사용하여 검출하였으며 반코마이신은 precursor ion m/z 725.0 ( $[M+2H]^{2+}$)와 product ion m/z 100.0을 사용하였다. 혈장에서 반코마이신의 검출한계는 1 nM이며 좋은 정확성과 정밀성을 보여주었다. 또한 혈장중에서 반코마이신의 정량범위는 $0.01{\mu}M$ - $100{\mu}M$이다. 혈장과 뇨중에서 반코마이신을 정량하는 이 분석방법은 약물동력학연구 및 관련연구에 성공적으로 적용되었다.

• 분석과학
• /
• 제21권4호
• /
• pp.316-325
• /
• 2008

연속흐름주입-수소화물생성-유도결합플라스마질량분석장치를 사용하여 바닷물시료중의 비소를 분석하였다. 두 종류의 바닷물표준시료인 CASS-4, NASS-5를 사용하여 측정값과 인증값을 비교함으로써 본 분석법의 정확성을 확인하였다. 분석결과 CASS-4의 경우 $1.17{\pm}0.07{\mu}g/L$ (인증값 $1.11{\pm}0.16{\mu}g/L$), NASS-5의 경우 $1.24{\pm}0.08{\mu}g/L$ (인증값 $1.27{\pm}0.12{\mu}g/L$)의 값을 얻었다. 이는 각각 독립적으로 5회 측정된 결과의 확장불확도로 표시된 결과이며 CASS-4의 경우 6.2%, NASS-5의 경우 6.8%이었으며 모두 인증값의 불확도 범위안에 있었다. 검량선의 기울기와 바탕값의 표준편차로부터 구한 $As^+$ (m/z=74.9216)의 검출한계는 0.01 ug/kg이었다. 검량선의 직선성은 매우 양호하였다. ($R^2=1$). DRC gas로 산소기체를 사용하여 $AsO^+$ (m/z=90.9165)로 검출하는 방법을 사용하여 결과를 비교하였으며 분석감도는 약 25배 정도 감소하였으나, 검량선의 직선성이 매우 잘 나타났으며, 분석결과도 $As^+$(m/z=74.9216)로 검출할 때와 동일한 결과를 얻을 수 있었다.

• 분석과학
• /
• 제17권2호
• /
• pp.117-129
• /
• 2004

본 연구에서는 극성이 높고, 휘발성이 낮아 GC나 GC/MS로 분석이 곤란한 환경매체 중의 아미트롤을 LC/ESI/MS를 사용하여 분석한 결과 다음과 같은 결론을 얻었다. 분자량이 84인 아미트롤은 LC/ESI/MS 방식에서는 m/z 85인$(M+H)^+$형태로 나타났으며, 피크강도는 30V에서 (SIR mode) 최대를 나타내었다. 질량 스펙트럼 비를 정성확인에 적용하기 위하여 실험한 결과 아미트롤은 m/z 85 와 m/z 58 이온으로 나타났으며, 50V에서 이 비는 1 : 7.03~7.58 로 나타났다. 동위원소 비를 이용한 정성확인은 isotope MS나 HR/MS가 주로 사용되나, 본 연구에서는 정성확인을 위한 보조수단으로 이용하고자 실험한 결과 아미트롤의 동위원소는 $86([M+H])^+$ 형태로 나타났으며, 시료에서(30V) m/z 85와 m/z 86의 질량 스펙트럼 비는 27.1~28.6 : 1(이론적 비 26.6 : 1)로 나타났다. 단계별 표준액을 시료의 전 처리 방법과 동일하게 처리하여 분석한 검량선의 직선성은 $y=1.09354e^6X+26947.2$이었으며, $r^2=0.99$로 나타났다. 분석의 정도관리를 위한 회수율검정과 반복 재현성을 알아보기 위한 실험에서 수질시료의 회수율은 77.64~83.44%, 토양시료에서는71.11~79.44%로 나타났으며, 각 농도 단계별 반복(5회)실험결과 상대표준편차 값은 10%이하를 나타내었다.

• Journal of Pharmaceutical Investigation
• /
• 제34권6호
• /
• pp.513-519
• /
• 2004

A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

• 한국농공학회지
• /
• 제20권1호
• /
• pp.4592-4598
• /
• 1978

The purpose of this research is to find out mathemetically an economical intake water depth in the design of head works through the derivation of some formulas. For the performance of the purpose the following formulas were found out for the design intake water depth in each flow type of intake sluice, such as overflow type and orifice type. (1) The conditional equations of !he economical intake water depth in .case that weir body is placed on permeable soil layer ; (a) in the overflow type of intake sluice, {{{{ { zp}_{1 } { Lh}_{1 }+ { 1} over {2 } { Cp}_{3 }L(0.67 SQRT { q} -0.61) { ( { d}_{0 }+ { h}_{1 }+ { h}_{0 } )}^{- { 1} over {2 } }- { { { 3Q}_{1 } { p}_{5 } { h}_{1 } }^{- { 5} over {2 } } } over { { 2m}_{1 }(1-s) SQRT { 2gs} }+[ LEFT { b+ { 4C TIMES { 0.61}^{2 } } over {3(r-1) }+z( { d}_{0 }+ { h}_{0 } ) RIGHT } { p}_{1 }L+(1+ SQRT { 1+ { z}^{2 } } ) { p}_{2 }L+ { dcp}_{3 }L+ { nkp}_{5 }+( { 2z}_{0 }+m )(1-s) { L}_{d } { p}_{7 } ] =0}}}} (b) in the orifice type of intake sluice, {{{{ { zp}_{1 } { Lh}_{1 }+ { 1} over {2 } C { p}_{3 }L(0.67 SQRT { q} -0.61)}}}} {{{{ { ({d }_{0 }+ { h}_{1 }+ { h}_{0 } )}^{ - { 1} over {2 } }- { { 3Q}_{1 } { p}_{ 6} { { h}_{1 } }^{- { 5} over {2 } } } over { { 2m}_{ 2}m' SQRT { 2gs} }+[ LEFT { b+ { 4C TIMES { 0.61}^{2 } } over {3(r-1) }+z( { d}_{0 }+ { h}_{0 } ) RIGHT } { p}_{1 }L }}}} {{{{+(1+ SQRT { 1+ { z}^{2 } } ) { p}_{2 } L+dC { p}_{4 }L+(2 { z}_{0 }+m )(1-s) { L}_{d } { p}_{7 }]=0 }}}} where, z=outer slope of weir body (value of cotangent), h1=intake water depth (m), L=total length of weir (m), C=Bligh's creep ratio, q=flood discharge overflowing weir crest per unit length of weir (m3/sec/m), d0=average height to intake sill elevation in weir (m), h0=freeboard of weir (m), Q1=design irrigation requirements (m3/sec), m1=coefficient of head loss (0.9∼0.95) s=(h1-h2)/h1, h2=flow water depth outside intake sluice gate (m), b=width of weir crest (m), r=specific weight of weir materials, d=depth of cutting along seepage length under the weir (m), n=number of side contraction, k=coefficient of side contraction loss (0.02∼0.04), m2=coefficient of discharge (0.7∼0.9) m'=h0/h1, h0=open height of gate (m), p1 and p4=unit price of weir body and of excavation of weir site, respectively (won/㎥), p2 and p3=unit price of construction form and of revetment for protection of downstream riverbed, respectively (won/㎡), p5 and p6=average cost per unit width of intake sluice including cost of intake canal having the same one as width of the sluice in case of overflow type and orifice type respectively (won/m), zo : inner slope of section area in intake canal from its beginning point to its changing point to ordinary flow section, m: coefficient concerning the mean width of intak canal site,a : freeboard of intake canal. (2) The conditional equations of the economical intake water depth in case that weir body is built on the foundation of rock bed ; (a) in the overflow type of intake sluice, {{{{ { zp}_{1 } { Lh}_{1 }- { { { 3Q}_{1 } { p}_{5 } { h}_{1 } }^{- {5 } over {2 } } } over { { 2m}_{1 }(1-s) SQRT { 2gs} }+[ LEFT { b+z( { d}_{0 }+ { h}_{0 } )RIGHT } { p}_{1 }L+(1+ SQRT { 1+ { z}^{2 } } ) { p}_{2 }L+ { nkp}_{5 }}}}} {{{{+( { 2z}_{0 }+m )(1-s) { L}_{d } { p}_{7 } ]=0 }}}} (b) in the orifice type of intake sluice, {{{{ { zp}_{1 } { Lh}_{1 }- { { { 3Q}_{1 } { p}_{6 } { h}_{1 } }^{- {5 } over {2 } } } over { { 2m}_{2 }m' SQRT { 2gs} }+[ LEFT { b+z( { d}_{0 }+ { h}_{0 } )RIGHT } { p}_{1 }L+(1+ SQRT { 1+ { z}^{2 } } ) { p}_{2 }L}}}} {{{{+( { 2z}_{0 }+m )(1-s) { L}_{d } { p}_{7 } ]=0}}}} The construction cost of weir cut-off and revetment on outside slope of leeve, and the damages suffered from inundation in upstream area were not included in the process of deriving the above conditional equations, but it is true that magnitude of intake water depth influences somewhat on the cost and damages. Therefore, in applying the above equations the fact that should not be over looked is that the design value of intake water depth to be adopted should not be more largely determined than the value of h1 satisfying the above formulas.

• Journal of Pharmaceutical Investigation
• /
• 제37권4호
• /
• pp.223-227
• /
• 2007

A rapid, simple and sensitive LC/MS/MS method for the determination of lercanidipine in human serum was validated and applied to the pharmacokinetic study of lercanidipine. Lercanidipine and internal standard, amlodipine, were extracted from human serum by liquid-liquid extraction with hexan-isoamyl alcohol (100: 1, v/v) and analyzed on a $Symmetry^{(R)}$ MS $C_{18}$ column with the mobile phase of acetonitrile-0.2% aqueous formic acid (70: 30, v/v). Using MS/MS with multiple reaction monitoring (MRM) mode, lercanidipine and amlodipine were detected without severe interferences from human serum matrix. Lercanidipine produced a protonated precursor ion ($[M+H]^+$) at m/z 612.3 and a corresponding product ion at m/z 280.0. Internal standard produced a protonated precursor ion ($[M+H]^+$]) at m/z 409.0 and a corresponding product ion at m/z 238.0. The ruggedness of this method was investigated using quality control (QC) samples. This method showed linear response over the concentration range of 0.05-20 ng/mL with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 mL of serum was 0.05 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the developed method ranged from 85.51 to 112.2% for lercanidipine with overall precision (% C.V.) being 3.56-13.1%. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of lercanidipine in human serum samples for the pharmacokinetic studies, demonstrating the suitability of the method.

• Steel and Composite Structures
• /
• 제51권3호
• /
• pp.225-241
• /
• 2024

For several reasons, cold-formed steel (CFS) beams are often manufactured with holes. Nevertheless, because of holes, the reduction in the web area causes a decrease in the bending strength. Edge stiffeners are presently added around the holes to improve the bending strength of flexural members. Therefore, this research studies CFSZ-beams with stiffened holes and investigates how edge stiffener affects bending strength and failure modes. Nonlinear analysis was carried out using ABAQUS software and the developed finite element (FE) model was verified against tests from previous studies. Using the verified FE model, a parametric study of 104 FE models was conducted to investigate the influence of key parameters on bending strength of Z- sections. The results indicated that the effect of holes is less noticeable in very thin Z-sections. Moreover, adding edge stiffeners around the holes improves the flexural capacity of Z-beams and sometimes restores the original bending capacity. Because the computational techniques used to solve the CFS buckling mode with stiffened holes are still unclear, a numerical method using constrained and unconstrained finite strip method (CUFSM) software was proposed to predict the elastic distortional buckling moment for a wide variety of CFSZ-sections with stiffened holes. A numerical method with two procedures was applied and validated. Upon comparison, the numerical method accurately predicted the distortional buckling moment of CFS Z-sections with stiffened holes.

• 수산해양기술연구
• /
• 제22권2호
• /
• pp.22-30
• /
• 1986

It is very important for a navigator on bridge to know the maneuverability of his ship sufficiently at sea. Generally, the data of a turning circle test have long been used to study and evaluate the maneuverability of a ship. But referring only the data of the turning circle test method, he can not evaluate his ship's maneuvering characteristics sufficiently. So nowaday the test method added Z test to turning circle test for more detail references is considered to be desirable. In this paper, the authors performed PAL test and Z test together in order to study the maneuverability of M. S.Pusan 403, training ship of the National Fisheries University of Pusan. According to the results of PAL test, the rudder effect in port rudder angle of the M. S. Pusan 403 was found to be more effective than that in starboard one, because her changing amounts of angular velocity, turning radius and tangent speed in port rudder angles were found to be larger than those of them in starboard rudder one in unsymmetry. The relation between her drift angle(.8) and rudder angle (0) was found to be changing with .8=0.640 in direct proportion. As it appeared that her calculated K'-values were smaller than the standard K'-values of different kinds of ships in accordance with her Z test, her turning ability was found to be lower. The running distance of a turn in her 10$^{\circ}$ Z test was about 8.3 times her own length and was found not to be exceeded the standard maneuvering distance, therefore she was considered to have good maneuverabilities synthetically.

• Wind and Structures
• /
• 제12권3호
• /
• pp.281-283
• /
• 2009

Marquardt method is used to estimate the aerodynamic parameters in urban area of Beijing City, China, including displacement length (d), roughness length ($z_0$) and friction velocity (u*) and drag coefficient. The surface drag coefficient defined as the ratio between friction velocity and mean wind speed is 0.125 in our research, which is close to typical urban area value. The averaged d and $z_0$ are 1.2 m and 7.6 m. d and $z_0$ change with direction because of the surface heterogeneity over urban surface and reach their maximum values at S-SW sector, this tendency agrees with the surface rough element distribution around the observation tower.

• 환경위생공학
• /
• 제19권4호
• /
• pp.25-33
• /
• 2004

Acrylamide, difficult to analyze by GC and GC/MS due to the polarity and low volatility, was analyzed by LC/ESI/MS in the study. Acrylamide its(molecular weight 71amu) showed m/z=72 $(M+H)^+$ and high peak intensity at 22V in SIR mode. The mass spectrum ratios of acrylamide for qualitative identification had m/z=72 in precursor ion and m/z=55 in products ion, respectively. Those ratios at 30V in SIR mode ranged from 1: 1.4 to 1:1.17 despite various acrylamide concentrations. The ion intensity ratios of acrylamide $(m/z=72,\; [M+H]^+)$ to acrylamide isotopes $(m/z=73,\;[M+H]^+)$ ranged from 100 : 3.57 to 100 : 3.92. The results verified theoretical mass spectrum ratio that was 100:3.82. The linearity of standard calibration curve was y : 520.584x + 1815.26 with $r^2=0.99.$ In quality assurance and quality control, the recovery rate ranged from 81.64 percent to 90.97 percent and relative standard deviation was less than $10\%$ with 5 repeated injections at individual standard calibration solutions. The method was applied to analyze acrylamide in food at grocery stores. Snacks made of potatoes showed the highest acrylamide concentration followed by products made of French fries, wheat, and corn.