荧光法直接测定环境水中邻羟基苯甲酸和苯酚混合物的含量

本文研究了用荧光分光光度法测定环境水中苯酚和邻羟基苯甲酸的含量,在pH＞11时直接测定邻羟基苯甲酸的含量,波长为λex/λem=289/338nm,检出限为3.4ng/mL,线性范围0-6.0μg/mL.在pH=6,波长为λex/λem=270/297nm测得苯酚含量,检出限为4.0ng/mL,线性范围在0-0.85μg/mL,回收率为98%-101%,结果满意.     

固相萃取-高效液相色谱测定污水中的地塞米松

建立固相萃取-高效液相色谱法测定污水中地塞米松含量的方法。水样经固相萃取柱萃取富集后进行HPLC分析,以甲醇:水=65:35(V/V)为流动相,色谱柱为Agilent C18柱(5μm,4.6mm×150mm),柱温30℃;流速为1mL/min;紫外检测波长为240nm。地塞米松在25—300ng/mL范围内线性关系良好(n=5,R2=0.9992),最低检测浓度为25ng/mL(S/N>10),回收率为98.36%,地塞米松的低、中、高的日内精密度与日间精密度RSD均小于3%。本法准确、灵敏,能较好的应用于污水中地塞米松的测定。     

浙产檵木叶中槲皮素和山奈酚的含量测定

建立用反相高效液相色谱法同时测定浙产檵木叶中槲皮素和山奈酚含量的方法.采用Eclipse XDB-C18柱;柱温:25℃;流动相为乙腈-0.4％磷酸水溶液(35 ∶ 65,V/V);流速1.0mL/min;检测波长360nm.结果表明,槲皮素、山奈酚在1-100ng/μL的范围内均具有良好的线性关系(r槲皮素=0.99...     

ICP-MS测定开口箭根茎中的27种金属元素

采用电感耦合等离子体-质谱(ICP-MS)法测定了湖北省长阳县乐园镇产开口箭根茎中27中金属元素的含量.其中13中金属元素V、Cr、Mn、Fe、Cu、Zn、As、Se、Mo、Ag、Cd、Tl、Pb等采用普通模式检测,14种金属元素Li、Be、B、Mg、Al、Co、Ni、Ga、Rb、Sr、Te、Ba、Bi、U等采用碰撞/反应池技术(CCT)模式测定,以消除样品溶液中潜在的干扰.实验条件下,Co、Ni、Cr、Zn、Se、Mo、Ag、Pb等8种金属元素未检出.方法检出限Fe为9.789ng/mL、Cr为2.691ng/mL,Zn为1.803ng/mL,B为2.076ng/mL,Mg为1.977ng/mL,Al为3.024ng/mL,Ni为1.824ng/mL,其它元素为0.003-0.921ng/mL,精密度的RSD为0.164％-9.933％,加标回收介于90.0％-110.0％之间.     

湿法消解-原子荧光光谱法测定人参皂苷中的重金属元素

采用原子荧光光谱法对由人参根、茎、花提取的人参皂苷进行重金属含量的测定,为生产厂家提供科学数据。结果表明As、Hg、Se、Cd元素分别在0—0.10μg/mL、0—1.0ng/mL、0—10ng/mL、0—1.0ng/mL范围呈良好的线性关系,检出限分别为0.17ng/mL、0.10ng/L、0.011ng/mL、0.61ng/L。此法操作简便,灵敏度高,测定结果令人满意。     

ICP-AES测定铜精矿中的Ag含量及与AAS的比较

铜精矿样品经盐酸、硝酸、氢氟酸、高氯酸分解完全后,用10％的盐酸溶液(V/V)定容至50mL容量瓶中,应用电感耦合等离子体-原子发射光谱法(ICP-AES)测定其中的银含量.该方法的加标回收率为95.4％-97.2％,相对标准偏差(RSD)为1.26％,线性范围宽,具有良好的准确性和精密度,测定结果与AAS法吻合.与AAS法相比较,ICP-AES法具有更宽的线性范围,受介质盐酸溶液浓度的影响较少,适合用来测定铜精矿中的Ag.     

HPLC测定兔眼房水中两性霉素B的含量

建立兔眼房水中两性霉素B含量测定的高效液相色谱方法,研究两性霉素B脂质体药膜的缓释作用。采用Hypersil C18（4.6mm×150mm,5μm）色谱柱,以甲醇：EDTA-2Na（5mmol/L）=80：20（V/V）为流动相,流速：1mL/min;柱温：室温;检测波长：405nm;进样量：20μL。结果表明两性霉素B在22.3—2450ng/mL范围内线性关系良好（r=0.9996）,房水中两性霉素B的平均提取回收率大于95%,日内RSD为1.05%。检出限为4ng/mL。该法简便、准确、可靠,适合两性霉素B的含量测定。     

ICP-AES、石墨炉原子吸收光谱法及X射线荧光光谱法测定土壤中钒的比较

研究了土壤中钒的3种测定方法,ICP-AES、石墨炉原子吸收光谱法和X射线荧光光谱法.其中ICP-AES选用谱线V 311.1nm,用干扰系数法,干扰系数用多个土壤标样的标准值和测定值的最小二乘法来确定;石墨炉原子吸收光谱法用新、旧石墨管(热解涂层),加与不加基体改进剂(硝酸镁)分别进行测试;X射线荧光光谱法样品无需前处理、无需做校准曲线,测定前仪器用自带校正钢片单点法进行校正.通过测试结果的比较得出:ICP-AES测定土壤标样中的钒,精密度高,准确度好,适合土壤中钒的实验室分析;石墨炉原子吸收光谱法灵敏度过高(高一个数量级),信号稳定性较差,对高温元素钒的测定最好加硝酸镁机体改进剂消除基体干扰且每只石墨管分析次数不超过100次;X荧光光谱法较适合于野外监测或土壤样品无损检测,操作方便快速.     

荧光分光光度法定量分析OP乳化剂

通过对OP(聚乙二醇辛基苯基醚)乳化剂的荧光光谱研究,发现其在304nm处产生较强的荧光.在pH 5.5的B-R缓冲溶液中,OP乳化剂的荧光强度与其浓度在一定范围内呈良好的线性关系,据此建立了一种新的高灵敏度的测定方法.在0.1-50.0μg/mL的浓度范围内,测定波长λex/λem=226nm/304nm的回归方程为:F=22.12C+9.825(C:μg/mL,r=0.9995),检出限为0.068μg/mL;测定波长λex/λem=276nm/304nm的回归方程为:F=90.08C-10.12 (C:μg/mL,r=0.9999),检出限为0.053μg/mL.采用此两组测定波长对同组样品进行测定,样品回收率均在96.5％以上,对测定结果进行F检验和t检验分析,得出两组数据之间无显著性差异.方法灵敏度高,抗干扰能力较强,可用于测定较复杂环境样品中微量OP乳化剂含量.     

氯酚红共振瑞利散射法测定残留氯霉素

建立了测定残留氯霉素的共振瑞利散射法.在pH 9.25的Tris-HCl缓冲溶液中,氯霉素与氯酚红相互作用后,共振瑞利散射显著增强,在407nm处呈现最高散射强度.氯霉素的质量浓度在0.030-0.260μg/mL范围内与ΔⅠRRS成正比,检出限(3Sb/S)为0.0020μg/mL.该法简便、快速、灵敏,可用于虾及奶粉中氯霉素残留测定.     

Detection of carcinoembryonic antigen using functional magnetic and fluorescent nanoparticles in magnetic separators

We combined a sandwich immunoassay, anti-CEA/CEA/anti-CEA, with functional magnetic (~80 nm) and fluorescent (~180 nm) nanoparticles in magnetic separators to demonstrate a detection method for carcinoembryonic antigen (CEA). Determination of CEA in serum can be used in clinical diagnosis and monitoring of tumor-related diseases. The CEA concentrations in samples were deduced and determined based on the reference plot using the measured fluorescent intensity of sandwich nanoparticles from the sample. The linear range of CEA detection was from 18 ng/mL to 1.8 pg/mL. The detection limit of CEA was 1.8 pg/mL. In comparison with most other detection methods, this method had advantages of lower detection limit and wider linear range. The recovery was higher than 94%. The CEA concentrations of two serum samples were determined to be 9.0 and 55 ng/mL, which differed by 6.7% (9.6 ng/mL) and 9.1% (50 ng/mL) from the measurements of enzyme-linked immunosorbent assay (ELISA), respectively. The analysis time can be reduced to one third of ELISA. This method has good potential for other biomarker detections and biochemical applications.     

载脂蛋白免疫复合物微粒的共振散射光谱研究及分析应用

在pH 6.8的Na₂HPO₄-NaH₂PO₄缓冲溶液中和聚乙二醇存在下,载脂蛋白A1(APOA1)、载脂蛋白B(APOB)与相应的抗体发生特异性结合,分别形成粒径约为180,140 nm的抗体抗原免疫复合物微粒,导致体系在340,470 nm处的共振散射峰增强。分别研究了pH、抗血清、聚乙二醇浓度、温育时间和共存物质的影响。在最佳条件下,APOA1浓度在8.4～430.0 ng·mL-1, APOB浓度在14.8～590.0 ng·mL-1范围内与其共振散射强度成良好线性关系,方法的检出限分别为6.2和7.0 ng·mL-1,用于定量分析血清中的APOA1与APOB, 获得满意结果。     

浊点萃取-分光光度法测定水环境中的痕量磷酸盐

建立了分光光度法测定水样中痕量磷酸盐的浊点萃取分离富集新体系。在酸性条件下,以抗坏血酸、钼酸铵作为磷钼蓝比色法测定磷含量的显色剂,酒石酸锑钾作为催化剂,形成稳定的磷钼蓝后,通过80℃水浴加热10m in,磷钼蓝被萃取到T rition X-100表面活性剂相并与水相分离。将表面活性剂富集相用0.5mL乙醇分散稀释,应用紫外-可见分光光度计进行400—1000nm范围内的波长扫描。在最佳条件下,测定的线性范围为0.3—180ng/mL,方法的检出限为0.73ng/mL,相对标准偏差（RSD）为2.8%。该法用于实际水样的富集和测定,结果令人满意。     

催化荧光法测定痕量亚硝酸根

在稀磷酸介质中 ,溴酸钾可氧化吖啶橙使之褪色并伴随着吖啶橙荧光强度的减弱 ,但反应速率较慢。痕量亚硝酸根的存在对该反应可起到显著的催化作用 ,使反应的灵敏度明显提高 ,体系的荧光猝灭程度加强。基于此采用固定时间法提出了一种灵敏度高、选择性好的催化荧光法测定痕量亚硝酸根的新方法 ,并研究了该方法的动力学条件。催化反应在λex/λem =4 4 6 / 5 0 5nm处 ,5 5℃水浴中进行 10min。反应可允许较大量的 2 0多种常见离子存在 ,同倍量的Fe3 ,Br-、I-不干扰。亚硝酸根的线性范围为 0 0 5～ 5ng·mL-1,方法的检出限为 0 0 12ng·mL-1。用于水体和土壤中痕量亚硝酸根的测定 ,结果满意。     

甲苯胺蓝共振光散射法测定纳克级脱氧核糖核酸

研究了吩噻嗪类染料甲苯胺蓝 (TB)与DNA作用的共振光散射光谱 ,在pH 1 0～ 1 1的范围内 ,加入DNA导致甲苯胺蓝共振光散射增强 ,在 35 0nm处 ,存在一共振光散射增强峰 ,其强度与DNA浓度呈线性关系 ,据此建立了一种测定DNA的共振光散射法。对于ctDNA ,方法的线性范围为 0～ 90 0ng·mL-1 ,检出限为6 75ng·mL-1 ,RSD为 3 7% ;对于fsDNA ,方法的线性范围为 0～ 90 0ng·mL-1 ,检出限为 2 99ng·mL-1 ,RSD为 5 6 % .已用于合成样品中DNA的测定     

核酸-桑色素-铝(Ⅲ)三元荧光体系的研究

基于核酸对桑色素 铝 (Ⅲ )配合物的荧光增强作用 ,以桑色素 铝 (Ⅲ )为荧光探针 ,考察该探针与核酸的结合反应 ,建立了新的准确测定核酸的方法 ,并研究了该三元荧光体系的作用机理。在 pH 8 5时 ,fsDNA ,ctDNA ,smDNA和 yRNA的浓度与桑色素 铝 (Ⅲ )的荧光强度成线性关系 ,响应范围分别为 0 2 5～1 5 0 ,0 2 5～ 2 0 0 ,0 10～ 1 6 0和 0 2 5～ 2 0 0 μg·mL-1,检测限 (3σ/K)分别为 3,2 ,2和 3ng·mL-1。测定了合成样品 ,回收率 93 3%～ 10 7 9% ,相对标准偏差小于 3 6 %     

Spectrofluorimetric Determination of Aliskiren in Tablets and Spiked Human Plasma through Derivatization with Dansyl Chloride

A simple and sensitive method has been developed and validated for the determination of aliskiren (ALS) in its dosage forms and spiked plasma. The method was based on the reaction of the drug with dansyl chloride in the presence of bicarbonate solution of pH 10.5 to give a highly fluorescent derivative which was measured at 501 nm with excitition at 378 nm in dichloromethane. Different experimental parameters affecting the development of the method and stability were carefully studied and optimized. The calibration curves were linear over the concentration ranges of 100–700 and 50–150 ng/mL for standard solution and plasma, respectively. The limits of detection were 27.52 ng/mL in standard solution, 4.91 ng/mL in plasma. The developed method was successfully applied to the analysis the drug in the commercial tablets and spiked plasma samples. The mean recovery of ALS from tablets and plasma was 100.10 and 97.81%, respectively. A proposal of the reaction pathway was presented.     

Conventional and First Derivative Synchronous Fluorometric Determination of Ethamsylate in Pharmaceutical Preparations and Biological Fluids. Application to Stability Studies

Two simple, accurate and highly sensitive spectrofluorometric methods were developed for the determination of ethamsylate (ETM). Method I is based on measuring the native fluorescence of ethamsylate in water at 354 nm after excitation at 302 nm. The calibration plot was rectilinear over the range of 0.05–1 μg/mL for ETM with limits of detection and quantitation of 7.9 and 26 ng/mL, respectively. Method II involved synchronous and first derivative synchronous fluorometric methods for the simultaneous determination of ethamsylate (ETM) and hydroquinone (HQ) which is considered as an impurity and/or acidic degradation product. The synchronous fluorescence of both the drug and its impurity were measured in methanol at Δ λ of 40 nm. The peak amplitudes (¹D) were estimated at 293.85 or 334.17 nm for ETM and at 309.05 nm for HQ. Good linearity was obtained for ETM over the ranges 0.1–1.4 μg/mL and 0.1–1.0 μg/mL at 293.85 and 334.17 nm, respectively. For HQ, the calibration plot was rectilinear over the range of 0.01–0.14 μg/mL at 309.05 nm. Limits of detection were 20, 2.01 ng/mL and limits of quantitation were 60, 6.7 ng/mL for ETM and HQ by method II, respectively. Both methods were successfully applied to commercial ampoules and tablets. The results were in good agreement with those obtained by the reference method. Method I was utilized to study the stability of ETM and its degradation kinetics using peroxide. The apparent first-order rate constant, half-life times and activation energy of the degradation process were calculated. Method I was further extended to the in-vitro and in-vivo determination of ETM in spiked and real plasma samples. The mean% recoveries were 99.57 ± 3.85 and 89.39 ± 5.93 for spiked and real human plasma, respectively.     

抗凝血酶Ⅲ的免疫共振散射光谱分析

在pH 7.2的Tris-HCl缓冲溶液中和聚乙二醇6000（PEG-6000）存在下,羊抗人抗凝血酶Ⅲ与抗凝血酶Ⅲ（AT-Ⅲ）发生免疫反应形成疏水性的免疫复合物微粒,导致体系的共振散射强度增强,在波长为368,491和538 nm处出现3个共振散射峰,其中491 nm处的峰最强。分别考察了pH、AT-Ⅲ和PEG-6000浓度、温育时间和温度、共存物质的影响。在选定条件下,AT-Ⅲ浓度在62.5～875 ng·mL-1范围内与491 nm处体系的散射强度呈良好的线性关系,其回归方程为ΔI_RS=62.5c+1.36,相关系数为0.996,检出限为29.4 ng·mL-1。该方法简便、灵敏和选择性好,用于人血中AT-Ⅲ含量的测定,结果满意,回收率在90.2%～108.9%之间。