奈替米星-刚果红分光光度法测定奈替米星

在pH4.5~6.0和pH1.9~3.1的酸性条件下,奈替米星(NTM)与刚果红(CR)反应,分别生成红色和蓝色离子缔合物,使刚果红红色溶液褪色。前者最大褪色波长位于500nm处,表观摩尔吸光系数(ε)为2.55×104Lmol-1cm-1;奈替米星在0.04~9.5mg/L浓度范围内,遵从朗伯比尔定律。后果者也使奈替米星在一定浓度范围内遵从朗伯比尔定律,但灵敏度不及前者。本文探讨了适宜的反应条件、主要分析化学性质及两种不同酸度范围内的络合比。所拟定的方法简便、快速,用于市售奈替米星药物及人尿、人血清中奈替米星含量的测定,结果满意。     

柱前衍生反相高效液相色谱-荧光检测法测定大鼠血浆中的奈替米星

建立了一种简便、灵敏的氯甲酸芴甲酯(FMOC-Cl)柱前衍生反相高效液相色谱-荧光检测血浆中奈替米星的新方法,同时研究了其药代动力学。对色谱条件进行了优化,采用ZORBAX Eclipse XDB-C8柱(150 mm×4.6 mm,5 μm),流动相为乙腈-水(体积比为85:15),流速为1.0 mL/min,荧光检测激发波长为265 nm,发射波长为315 nm,得到奈替米星的平均加标回收率为96.62%～100.84%(n=3),对奈替米星检测的线性范围为0.045～8.88 mg/L,相关系数为0.9993,方法的日内与日间精密度分别低于3%与3.5%,最低检出限(S/N=3)与定量限(以3倍检出限计)分别为0.01和0.03 mg/L。方法简便、快速、灵敏,样品用量少(30 μL奈替米星血浆溶液已能满足该药含量的测定以及药物代谢的研究),为大鼠体内奈替米星的药代动力学研究提供了可靠的分析手段。     

高效液相色谱-共振瑞利散射光谱法测定大鼠血清中的奈替米星

建立了高效液相色谱-共振瑞利散射光谱联用测定大鼠血清中奈替米星的方法.采用的色谱条件为:以C18柱为分离柱,以甲醇(含0.22%三氟乙酸)-20 mmol/L醋酸钠水溶液(8∶92,v/v)为流动相进行等度洗脱.以滂胺天蓝为分子探针,奈替米星在柱后与滂胺天蓝结合生成离子缔合物,产生强烈的共振瑞利散射信号,荧光检测器在激...     

大孔阳离子交换树脂对奈替米星的吸附研究

通过正交实验合成了9种大孔弱酸性阳离子交换树脂,筛选出具有最大动态饱和吸附量的FB-1树脂.采用红外光谱和热重分析的方法对其表征,并研究其对奈替米星的吸附及解吸性能,结果表明:该树脂对奈替米星的吸附符合Langrnuir吸附:用氨水做洗脱剂,0.3mol/L和0.4mol/L的氨水解吸率均达95%以上.FB-1与HD-2树脂比较:动态吸附量FB-1为398.0mg/mL湿树脂、HD-2为232.1mg/mL湿树脂;0.3mol/L氨水解吸,前者解吸率较后者高约15%.     

荷移分光光度法测定奈替米星

<正>奈替米星是一种半合成氨基糖苷类抗生素,抗菌谱广活性高,对肠杆菌科细菌如大肠杆菌、克雷伯菌属、肠杆菌属及变形杆菌属等具有良好的抗菌作用。目前,奈替米星的检测方法有分光光度法[1-2]、散射光谱法[3]、高效液相色谱法[4-5]、薄层色谱法[6]和高效毛细管电泳法[7]等。本工作利用水杨基荧光酮与奈替米星发生荷移反应生成稳定的荷移络合物,其最大吸收波长512nm,比试剂的最大吸收波     

头孢曲松钠与1,2-萘醌-4-磺酸钠的光度分析及应用

建立了用1,2-萘醌-4-磺酸钠(NQS)作为显色剂,分光光度法测定头孢曲松钠的新方法。在pH=13.0的缓冲溶液中,NQS与头孢曲松钠发生亲核取代反应生成1∶1的红褐色配合物,其最大吸收波长488nm。方法线性范围为2.4~168mg/L,相关系数r=0.9993,检出限为1.3mg/L。该法成功应用于针剂中头孢曲松钠含量的测定,回收率在98.2%~101.6%。     

1,2-萘醌-4-磺酸钠体系分光光度法测定头孢他啶

建立了用1,2-萘醌-4-磺酸钠(NQS)作为显色剂分光光度法测定头孢他啶(ceftazidime)的新方法.在pH 13.0缓冲溶液中,NQS能直接与头孢他啶发生亲核取代反应生成红褐色化合物,其最大吸收波长为484 nm.头孢他啶在2.98～127.3 mg/L浓度范围内与吸光度呈良好线性关系,线性回归方程A=0.0...     

奈替米星与依文思蓝的光度分析研究

硫酸奈替米星是半合成的一种较新的氨基糖苷类抗生素,由西梭米星乙酰化而成,它不但全面保留了西梭米星的体内抗菌活性,同时提高了西梭米星对钝化酶的耐受性,其抗菌谱广,活性高,耳、肾毒性较其他同类药小,现已广泛用于国内外临床[1-3]。对奈替米星的测定方法,目前已报道的主要有     

1,2-萘醌-4-磺酸钠体系分光光度法测定磺胺甲噁唑

采用1,2-萘醌-4-磺酸钠体系分光光度法测定磺胺甲噁唑(SMZ)。磺胺甲噁唑与1,2-萘醌-4-磺酸钠在pH=10.0的缓冲溶液中发生亲核取代反应生成橙红色的产物,组成比为1:1,最大吸收波长λ=476 nm;表观摩尔吸光系数ε=6.44×103L/(mol.cm);SMZ浓度在0.2~60 mg/L范围内呈良好的线性关系;线性回归方程为A=0.02452 0.02301C(mg/L),线性相关系数r=0.9991;检出限为0.08 mg/L;RSD为0.25%(20 mg/L,n=11);平均回收率为98.7%以上。优化了对磺胺甲噁唑的测定条件。初步探讨了反应机理,应用拟定的方法测定磺胺甲噁唑的含量,与药典法相比,结果满意。     

4-(5-氯-2-吡啶)-偶氮-1,3-二氨基苯显色光度法测定钯(Ⅱ)

研究了4-(5-氯-2-吡啶)-偶氮-1,3-二氨基苯(5-Cl-PADAB)与Pd的显色反应,在0.48 mol/L H3PO4介质和100℃水浴条件下,5-Cl-PADAB与Pd(Ⅱ)反应生成2:1稳定络合物,其最大吸收波长为570nm,表观摩尔吸光系数为6.39×104 L.mol-1.cm-1。结果表明:Pd含量在0～1.2 mg/L内符合比尔定律,方法已用于矿样中微量Pd的测定,结果与AAS法相符。样品分析结果的相对标准偏差小于4%,加标回收率为98.5%～103.0%。     

Bestimmung von Netilmicin im Serum mit dem Substrate-Labelled Fluorescent Immunoassay (SLFIA)

Ohne Zusammenfassung

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Determination of Netilmicin in serum by means of the substrate-labelled fluorescent immunoassay (SLFIA)

     

可溶性聚酰亚胺电化学反应机理的研究

本文研究了三种可溶性聚酰亚胺（ＰＩ）在机溶剂和水溶液中的电化学行为，发现ＰＩ在有机溶剂中的电化学行为明显不同于水溶液，利用红外光谱技术才半经验发子轨道计算方法，结合电化学测试的结果，确证了ＰＩ的电化学反应的机理。     

Influence of the Position of the Connecting Spacer of the Chromophore on the Nonlinear Optical Response

A new chromophore, C1 , based on a similar DπA‐structure as in the FTC ‐chromophore but with a hydroxyalkyl spacer perpendicular to the direction of the dipole moment was synthesized. Both chromophores and the CLD ‐chromophore were used to prepare high T_g nonlinear optical vinyl polymers. The influence of the position of the spacer on the DπA‐system on the NLO response of the resulting polymers was investigated.

     

Determination of the mechanism of the oxidation of the trichloromethyl radical by the photolysis of chloral in the presence of oxygen

The photooxidation of chloral was studied by infrared spectroscopy under steady-state conditions with irradiation of a blackblue fluorescent lamp (300 nm < λ < 400 nm, λ_max = 360 nm) at 296 ± 2 K. The products were hydrogen chloride, carbon monoxide, carbon dioxide, and phosgen. The kinetic results reveal that the reaction proceeds via chain reaction of the Cl atom: The results lead to the conclusion that mechanism (B) is confirmed to be more likely than mechanism (A), which was favored at one time by Heicklen for the mechanism of the oxidation of trichloromethyl radicals by oxygen molecules: The ratio of the initial rates of CO and CO₂ formation gave k₇/k₆ = 4.23M^?1, and the lower limit of reaction (5) was found to be 3.7 × 10⁸M^?1 sec^?1.     

An improvement of the resolution of the identity approximation for the formation of the Coulomb matrix

A straightforward modification of the resolution of the identity (RI) approximation to the Coulomb interaction is described. In the limit of basis sets that are dominated by high angular momentum functions the observed speedups in realistic test systems reach a factor of 2 compared to the standard RI algorithm, and a factor of up to 300 compared to the standard algorithm to form the Coulomb matrix. More moderate savings on the order of 0-20% are obtained for the more commonly used smaller basis sets. A series of test calculations is reported to illustrate the efficiency of the algorithm.