基于金沉积质量放大黄嘌呤压电传感技术研究

黄嘌呤(Xanthine,XA)是人体内嘌呤核苷酸分解代谢的中间产物,其在人体体液中含量的变化,可充分反映出人体内免疫、代谢等机能的状况.因此,人体体液中黄嘌呤含量的测定,在医学临床上具有重要意义.     

尿酸在聚亚甲基蓝修饰金电极上的电化学及电化学动力学性质

尿酸(Uric acid,UA)是人体内嘌呤核苷酸分解代谢过程中的最终产物.体液中尿酸的含量变化可以充分反映出人体新陈代谢、免疫等机能状况,同时也可间接反映出与嘌呤代谢的有关疾病[1].     

聚邻氨基对酚磺酸修饰电极测定尿酸

尿酸(UA)是核蛋白和核酸的代谢产物,人体内尿酸的水平与肝脏疾患[1]、肾病[2]以及心血管疾病[3]等有着密切的关系.因此,对人体体液中尿酸的定量分析无论在药物控制方面还是在临床诊断方面都具有重要意义.     

银掺杂聚L-半胱氨酸修饰电极测定尿酸

尿酸(UA)是人体内嘌呤代谢最终产物,它在人体体内含量的变化可直接导致某些疾病的发生.因此,对尿酸的化学检测、尤其是人体体液中的含量测定,在临床医学中具有较大的现实意义.     

离子色谱-电导检测法测定不同乳制品中硫氰酸盐

建立了离子色谱-电导检测分析不同类型乳制品中硫氰酸盐(SCN-)污染物的方法,重点研究了不同形态样品如固态类(奶粉)、液态类(牛奶)、凝固态类(凝固型酸奶)和半流质态类(炼乳)等乳制品中的硫氰酸盐前处理方法,采用丙酮作为蛋白沉淀剂,有效实现了对各类样品中蛋白质的沉淀和对硫氰酸盐的提取,避免了以往采用乙腈处理样品时容易分层的弊端,方法在0～5.0mg/L浓度范围内具有良好的线性关系,相关系数r为0.9997(n=6),方法检出限(LOD)为0.15～0.5μg/g,方法回收率为95.0%～105.0%,相对标准偏差(RSD)为1.4%～5.6%(n=3)。     

层状氢氧化镁铝焙烧产物对SCN-的吸附性能

研究了层状氢氧化镁铝焙烧产物对SCN-的吸附行为,考察了焙烧温度、吸附温度、时间、pH值等因素对吸附的影响.在SCN-初始浓度为25 mg/L,温度为40℃,焙烧物投加量为2 g/L,pH值为6的条件下,4 h达到吸附平衡,SCN-脱除率可达96.91%.吸附过程符合Langmu ir等温方程式,主要是单分子层的吸热吸附.     

超高效液相色谱-高分辨质谱法检测合成大麻素JWH-073在人肝微粒体中的Ⅰ相代谢产物

应用超高效液相色谱-高分辨质谱法检测合成大麻素JWH-073在人肝微粒体中的Ⅰ相代谢产物,用肝微粒体体外温孵法制备了加入JWH-073的人肝微粒体,从中了解JWH-073在人体内的代谢过程。JWH-073在人肝微粒体中共产生11种Ⅰ相代谢产物,其代谢途径为羟基化、羧基化、脱烷基化和羰基化,其中羟基化为主要途径,羟基化代谢产物有6种。根据代谢方式、代谢发生的位点及代谢产物的响应强度,推荐羟基化代谢产物(编号M4)作为JWH-073在人体尿液中的中毒标记物。在实际工作中仍需要收集人体尿液样品,通过筛查对比其中的主要代谢产物,最终确认JWH-073的代谢标记物。     

色谱-质谱联用技术在代谢组学中的应用

代谢组学是对生物体受外部刺激所产生的小分子代谢产物的变化或其随时间的变化进行研究的一门学科,以实现对体液、细胞以及组织提取物等复杂的生物样本中所有代谢产物的定性和定量分析为研究目标。色谱-质谱联用技术在代谢组学的研究中已显示出极大的发展潜力。本文主要综述近年来代谢组学研究中涉及的色谱-质谱联用技术及其数据处理方法,重点介绍各种分离技术的特点及其在应用中的关键问题,并对其在代谢组学应用中的未来发展给予展望。     

以双水杨醛缩二氨基硫脲合铜(Ⅱ)为载体硫氰酸根离子选择性电极的研究及其应用

以双水杨醛缩二氨基硫脲合铜(Ⅱ)[Cu(Ⅱ)-ATBSAD]为中性载体制备PVC膜电极,该电极对SCN-具有优良的电位响应特性。采用紫外光谱技术和交流阻抗技术研究了该电极对SCN-的响应机理。电极在磷酸盐缓冲溶液(pH5.0)中,SCN-浓度在1.0×10-1～1.4×10-7mol/L范围内呈近能斯特响应;斜率为-56mV/pSCN-(26℃);检出限为5.6×10-8mol/L。Cu(Ⅱ)-ATBSAD载体膜电极对SCN-具有较好的选择性,一些常见阴离子对电极的干扰较小。将此电极用于废水中硫氰酸盐含量的测定,结果与高效液相色谱法一致。     

钨的萃取分光光度法

硫氰酸盐比色法测定钨的干扰元素主要是钼。据报导,含氧类有机溶剂(如酯、醚、醇和酮类等)都能萃取钨和钼的硫氰酸盐络合物,而非极性有机溶剂(如苯、卤代烷烃、烷烃类等)都不萃取钨和钼的硫氰酸盐络合物,从而可以适当调整混合溶剂的比例,既定量萃取钨,又可分离大量钼。我们在文献[1]的基础上,用环己烷-醋酸丁酯萃取W-CNS,经实     

光化学-荧光分析法研究(Ⅷ)——波长扫描-反应速差分析法

提出了波长扫描-光化学反应速差荧光分析同时测定双组分的方法,以核黄素的光分解反应和甲萘醌的光还原反应为例考察了方法的可行性.结果表明,核黄素、甲萘醌浓度分别在(0～1.20)μg/mL和(0～2.70)μg/mL范围内呈良好的线性关系(γ为0.999和0.998).检出限分别为0.22ng/mL和2.6ng/mL(n=11).平均回收率分别为101%、99%.     

抑制荧光动力学法测定环境中痕量对硝基苯胺

在硫酸介质中,痕量对硝基苯胺对溴酸钾氧化罗丹明6G使其荧光猝灭具有抑制作用,由此建立了动力学荧光法测定痕量对硝基苯胺的分析新方法。考察了温度、反应时间、各种试剂条件对抑制反应的影响。在最佳实验条件下,方法线性范围为12~160 ng/mL,检出限为10.08 ng/mL。该方法应用于环境水样、土壤、大气等实际样品测定,回收率为96.8%~104.7%。     

抑制动力学荧光法测定痕量氟

在酸性介质中,利用氟离子对Fe(Ⅲ）催化H2O2氧化罗丹明6G使其荧光猝灭的抑制作用,建立了动力学荧光法测定痕量氟离子新方法,方法的线性范围为0.020-0.180μg/mL,检出限为8.70ng/mL。本法已用于牙膏中氟的含量测定。     

A highly sensitive fluorimetric method for the determination of fluoride in biological material with Al3+-calcein complex

A highly sensitive fluorimetric method for the determination of fluoride was established. The method was based on quenching of the fluorescence of the Al3+-calcein complex in CCl3COOH-CH3COOK buffer solution by fluoride. The fluorescence emission was measured at lambdaex/lambdaem 480/503 nm, and the experimental variables and interference in this determination were studied. The linear calibration range was 0.8 ng/mL to 150 ng/mL and the detection limit was 0.2 ng/mL. The method was applied to determine fluoride in biological materials. The recovery was in the range of 96.3% to 104.7% and the relative standard deviation was 4.6%. The results obtained from the certified reference material by the present method agreed with the certified values.     

基于痕量联苯胺阻尼作用的荧光光度分析

在HCl介质中，联苯胺的存在对KBrO3氧化吡咯红反应有抑制作用，据此建立了测定痕量联苯胺的荧光动力学新方法。对方法的介质条件、试剂用量、干扰物质影响进行了系统研究。在最佳实验条件下，方法的线性范围为30～400ng／mL，检出限为14．4ng／mL，对11份浓度为80ng／mL，300ng／mL的联苯胺标准溶液进行平行测定，相对标准偏差分别为2．1％和1．2％。本法用于塑料和雨水中联苯胺的测定，回收率为97．8％～102．1％。     

Determination of vitamin B12 in pharmaceutical preparations by a highly sensitive fluorimetric method

A fluorimetric method for the determination of vitamin B12 has been developed. The fluorescence emission was measured at lambda(ex)/lambda(em)275/305 nm in phosphate buffer solution (pH 7.0), and the experimental variables and possible interference were studied. The linear calibration range was 1.000 ng/mL to 100.0 ng/mL with a correlation coefficient of 0.9994 and a detection limit of 0.1 ng/mL. The method is rapid, simple and highly sensitive. It was used to determine vitamin B12 in pharmaceutical preparations. The recovery was 96%-98% and the relative standard deviation was in the range of 1.8%-2.7%. The results agreed with those obtained by spectrophotometry.     

光化学荧光分析法研究(Ⅵ)——混合色素的光化学速差动力学荧光分析法测定

以光化学荧光衍生化法测定苋菜红(AM)和直接耐晒嫩黄5GL(DY)2种偶氮色素,研究了同时测定这2种色素混合物的光化学速差动力学荧光分析的原理和方法。AM和DY的浓度分别在0～220ng/mL和0～120ng/mL范围内呈良好的线性关系,相关系数皆为0.999,检出限为0.64ng/mLAM和0.045ng/mLDY。相对标准偏差分别为1.6%(n=8)和1.8%(n=7)。该法用于人工合成混合样品的测定效果良好。     

Kinetic Spectrophotometric Determination of Trace Amounts of Nitrite by Catalytic Reaction between Methylthymol Blue and Bromate

A kinetic spectrophotometric method for determination of trace nitrite in two dynamic ranges (2–100 and 100–500 ng/mL) based on its catalytic effect on the reaction between methylthymol blue and potassium bromate in acidic (sulfuric acid) media is described. The reaction was monitored spectrophotometrically by measuring the decreasing color of methylthymol blue at 437 nm by the fixed‐time method of 4.0 min at 30°C. The detection limit is 0.6 ng/mL, and the relative standard deviations for 50.0 and 250.0 ng/mL nitrite are 1.6% and 1.3%, respectively. The method was used for the determination of nitrite in water samples.     

Kinetic spectrophotometric determination of traces of iron(II)

A simple method for the selective and sensitive kinetic spectrophotometric determination of iron (II) is described. The method is based on the oxidation reaction of reduced phenolphthalein by periodate in alkaline media. The change in absorbance was measured using the fixed time method. The effect of different variables on the reaction was investigated and optimum conditions were obtained. The calibration curve was linear in the range 50–3000 ng/mL, and a detection limit of 17 ng/mL was obtained. The relative standard deviation of ten replicate determinations of 200 ng/mL of Fe(II) was 1.2%. The determination of Fe(II) in the presence of a 50-fold amount of Fe(III) could be carried out. This article was submitted by the authors in English.