三甲氧基苯基荧光酮光度法测定生物样品中铅

研究了微乳液介质中,在pH91时,铅与三甲氧基苯基荧光酮(TMPF)显色生成稳定的1∶2配合物,在565nm处摩尔吸光系数为532×104L·mol-1·cm-1,铅含量在0～15μg·mL-1范围内符合比耳定律。巯基葡聚糖凝胶是一种将巯基基团引入葡聚糖骨架上的新型离子吸附剂,其吸附容量大,洗脱容易,机械性能好。采用巯基葡聚糖凝胶分离富集,消除了共存离子的干扰,显著提高了分析方法的选择性。测定了血样、发样和尿样中的痕量铅,结果令人满意。     

对硝基酚分光光度法测定氯氮卓的含量

本文主要研究在硼砂水溶液中 ,氯氮卓与对硝基酚发生荷移反应 ,生成稳定的 1∶ 1络合物。络合物的最大吸收波长为 4 35 nm,表观摩尔吸光系数 ε=3.83× 10 3L·mol-1·cm-1。基于以上反应 ,本方法测定氯氮卓药物制剂含量与文献值基本一致 ,回收率为 99.61%— 10 0 .10 % ,相对标准偏差为 0 .64%     

Spectrophotometric Determination of Certain Cephalosporins Using Ferrihydroxamate Method

Cephalexin, cefixime, ceftriaxone and cefotaxime were determined spectrophotometrically in the pure form and in pharmaceutical formulations by using ferrihydroxamate method. Reaction optimization with respect to reaction time and temperature has been investigated. Influence of the presence of ester functional group on the determination of cephalosporins as ß-lactams under conditions optimized was evaluated. Using cefotaxime sodiume as model drug with ester functional group, it was shown that proposed method gives equally acurate and precise results even in the presence of ester functional group.     

巯基葡聚糖凝胶分离富集微乳液增敏三甲氧基苯基荧光酮光度法测定痕量铜

研究在微乳液介质中, pH 10.40时, 铜与三甲氧基苯基荧光酮(TM-PF)显色生成稳定的1∶2配合物, 在552 nm 处摩尔吸光系数为1.46×105 L·mol-1·cm-1, 铜含量在0～0.6 μg·mL-1 范围内符合比耳定律,引入微乳液介质,显著改善了铜的显色条件,使体系灵敏度提高。采用吸附容量大,而机械性能好的巯基葡聚糖凝胶分离富集,消除了共存离子的干扰,降低了测定体系的检出限。测定了血样、尿样、水样和矿石样品中铜的测定,相对标准偏差低于4.8%,回收率为94.2%～106%。     

四氯对苯醌荷移分光光度法测定甲氧苄啶的含量

在乙醇溶液中甲氧苄啶与四氯对苯醌发生荷移反应 ,形成稳定的 1∶ 1络合物 ,最大吸收波长位于4 34.8nm,表观摩尔吸光系数为 ε=7.4 5 3× 10 2 L·mol-1·cm-1,甲氧苄啶含量在 30— 5 0 0 μg/m L范围内符合比耳定律 ,回收率为 99.82 %— 10 0 .3% ,相对标准偏差为 1.6 % (n=5 )。     

酸性品红分光光度法测定蛋白质的研究

在ＰＨ１．８的ＫＨ２ＰＯ４－Ｈ３ＰＯ４缓冲介质中,蛋白质与酸性品红结合使染料的吸光度下降。蛋白质浓度Ｃ在０．４０－４．００ｍｇ·Ｌ＾－１和８．００－４０．００ｍｇ·Ｌ＾－１范围内,吸光度的降低与蛋白质浓度（Ｃ）呈线性关系,回归方程分别为△Ａ＝０．０１４０Ｃ＋０．０５３４和△Ａ＝０．０１０９Ｃ＋０．０８９５,相关系数ｒ依次为０．９９６５和０．９９９３,方法用于奶粉和麦片中蛋白质的测定,结果满意。     

钼酸铵和乙基罗丹明B光度法测定微量钯

本法研究了在聚乙烯醇（PVA）存在下，色与钼酸铵和乙基罗丹B（ERB）反应形成的有色离子缔合物用于微量钯的光度法测定。缔合物的最大吸收位于580nm，表观摩尔吸收系数ε为2.13×10^5L·mol^-1·cm^-1，钯量在0－5.5μg/25mL范围内服从比耳定律。体系至少稳定140h，检出限(3σ）8.64μg/L(n=11），对0.20mg/L Pd（Ⅱ）测定的相对标准偏差为2.66%(n=12)。缔合物的摩尔比为Pd：ERB＝1：4。考查了50多种共存离子的影响。本法用于炭基和名基催化剂中微量色的测定，结果满意。     

同步荧光光谱法测定水中痕量萘和菲

同步荧光法具有选择性好、灵敏度高、干扰少等特点,可用于多组分多环芳烃混合物的同时测定,本文建立了恒定波长同步荧光光谱法同时测定水中萘和菲的新方法。研究了萘和菲在不同溶剂中的荧光光谱特性,确定了同步荧光的最优波长差。当Δλ=100 nm,萘和菲激发波长(λ_ex)分别为220.2和248.8 nm时,在0.5～25.0 μg·L-1浓度范围内,荧光强度与浓度呈现良好的线性关系,相关系数分别为0.999 5和0.999 7;萘和菲检出限均低于0.03 μg·L-1,回收率在98.0%～101.5%。该方法方便快捷,预处理简单,可用于水中萘、菲的快速测定。     

Determination of Enoxacin Using Tb Composite Nanoparticles Sensitized Luminescence Method

In our study, terbium-acetylacetone (Tb-acac) composite nanoparticles have been prepared under vigorous ultrasonic irradiation. The nanoparticles are water soluble, stable and have extremely narrow emission bands and high internal quantum efficiencies. They were used as fluorescence probes in the determination of enoxacin (Enox) based on the fluorescence enhancement of nanoparticles through fluorescence resonance energy transfer (FRET). The influence of buffer solution on the fluorescence intensity was investigated. Under the optimum conditions, the fluorescence intensity of the Tb-acac-Enox system is linearly proportional to the Enox concentration in the Enox concentration range of 2 × 10⁻⁷–1 × 10⁻⁴ M. The correlation coefficient for the calibration curve was 0.9976. The limit of detection as defined by IUPAC, C _LOD = 3S _b/m (where S _b is the standard deviation of the blank signals and m is the slope of the calibration graph) was found to be 3 × 10⁻⁸ M. The relative standard deviation (RSD) for six repeated measurements of 1 × 10⁻⁴ M Enox was 1.35%. The method was applied to the determination of Enox in pharmaceutical formulation and recovery results were obtained from urine samples.     

流动注射固相预富集原子吸收光谱法测定铁和钴

研究了用邻菲罗啉为配合剂,Ｃ１８键合硅胶为固相富集材料,流动注射在线固相萃取预富集火焰原子吸收法测定痕量铁和钴的方法。该方法自动化程度高,选择性强。经３０ｓ预富集、方法的采样速度达９０次／ｈ,铁和钴的富集倍数分别达１９倍和２０倍,检出限分别达３μｇ／Ｌ和６μｇ／Ｌ。     

聚乙二醇-钍试剂-硫酸钠体系中非有机溶剂萃取光度法测定铁

本文研究了铁（Ⅲ）－ＰＥＧ（聚乙二醇－２０００）－钍试剂－Ｎａ２ＳＯ４体系的析相光度法并应用于测定Ｆｅ（Ⅲ），最适酸度为４．６（ＮａＡｃ－ＨＡｃ）缓冲溶液，其络合物的最大吸收位于５６６ｎｍ，表观摩尔吸光系数为８．０６×１０３Ｌ·ｍｏｌ－１·ｃｍ－１。Ｆｅ（Ⅲ）浓度在０—３０μｇ·ｍＬ－１范围内服从比耳定律，该方法用于发样中铁的测定，获得了满意结果     

析相光度法测定铁(Ⅲ)的研究

本研究了铁（Ⅲ）－ＰＥＧ（聚乙二醇－２０００）－铬锖Ｒ－Ｎａ２ＳＯ４体系的上光度法并应用于测定Ｆｅ（Ⅲ）。最适酸并为４．５￣６．５（ＮａＡｃ－ＨＡｃ）缓冲溶液,其络合物的最大吸收位于５６０ｎｍ,表观摩尔吸光系数为５．３６×１０＾４Ｌ·ｍｏｌ＾－１·ｃｍ＾－１,Ｆｅ（Ⅲ）浓度在０￣４μｇ范围内服从比尔定律,铁与铬菁Ｒ形成组成为１：２的稳定络合物。该方法用于蔡叶中铁的测定,获得了满意的结果。     

析相光度法测定铜（Ⅱ）的研究

本文研究了Ｃｕ－ＰＥＧ－ＤＤＴＣ（铜试剂）（ＮＨ４）２ＳＯ４体系的析相光度法并应用于测定Ｃｕ。最宜酸度为３．６－９．０（ＮａＡｃ－ＨＡｃ，ＮＨ４Ｃｌ－ＮＨ３．Ｈ２Ｏ）缓冲溶液，其络合物的最大吸收位于４５０ｎｍ，表观摩尔吸光系数为９．０５×１０＾３Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，Ｃｕ浓度在０－３０μｇ／Ｌ范围内服从比耳定律，铜与ＤＤＴＣ形成组成为１：２的稳定络合物。该方法用于铝合金中铜的测定，获得了满     

8-羟基喹啉快速共沉淀分离富集原子吸收光谱法测定啤酒中的Cu和Pb

研究了用8-羟基喹啉-Mg(Ⅱ)共沉淀体系,以Mn(Ⅱ)为内标,快速共沉淀分离富集啤酒中的铜和铅,并用火焰原子吸收光谱(FAAS)测定的方法。共沉淀受pH值、载体镁和内标锰用量的影响。结果显示在pH为9的条件下,能够定量共沉淀试样中的铜和铅。当试液为100 mL时,方法的检出限分别为铜6.28×10-3 μg·mL-1,Pb 2.26×10-2 μg·mL-1回收率为97.6%～103.0%,基本消除了基体干扰,取得了较为满意的结果。该方法无需收集全部沉淀,与传统的共沉淀方法比较,克服了收集沉淀费时的缺点。方法快速、简便、重现性好。     

Spectrophotometric and Spectrofluorimetric Determination of Ofloxacin

Two methods are presented for the analysis of ofloxacin. The first method is based on the application of A_max, ΔA, first and second derivative techniques for its determination in bulk powder, tablet form, and in urine. The use of absorbance and derivative maxima ratios as purity indices has been discussed. The second depends on the fluorescence characteristics of ofloxacin in acidic solutions. The spectrofluorimetric method is 10 times more sensitive than the spectrophotometric one. The accuracy and reproducibility of the methods were shown by the within day and between day coefficient of variation (less than 3%).     

Determination of Lead in MIBK Extracts Using a Modified Long Path Atomic Absorption Cell

A long path atomic absorption cell has been modified to achieve high sensitvity in the determination of lead after MIBK extraction. This was achieved by using thermal insulation of the absorption cell and positioning the burner at an optimum angle. Insertion of rings inside the cell and oxygen supply line reduced the background noise to a low level while producing high sensitivities. This resulted in a marked improvement in detection limits for some metals in aqueous solution.     

DPD光谱分析法快速测定水中游离氯浓度

采用分光光度计测量了游离氯溶液与氨基-N,N-二乙基苯胺(DPD)试剂反应后溶液在可见光范围内的吸收光谱。讨论了吸收光谱的峰值波长随时间的变化关系,通过对不同浓度溶液的实验,得出了光谱测量误差,此误差值小于0．04％,并采用非线性数据拟合方法对实验数据进行了分析,找出了游离氯浓度与光透过率之间的关系式并给出了评价参数。