塞曼石墨炉原子吸收法直接测定血清中的硒

采用硝酸钯为硒的基体改进剂，用塞曼效应扣除背景，对消化后的血样直接进行测定。该法的检出限为6．0ng/mL，线性范围10ng/mL－136ng/mL，回收率为94．8％－102．5％。     

电热原子吸收法测定人发中硒时不同改进剂的研究

对于生物体中硒的测定,国内外已有大量报道,所用方法也相当广泛。本文利用石墨炉原子吸收对人发中硒的测定进行了研究;对使用较多的两种硒的基体改进剂:铜与镍的作用与效果进行了研究,发现铜较镍在某些方面更为优越。当选用100 μg/mL的铜作改进剂时,硒的特征浓度为0.13 ng/1％abs,测定精度为3.4％～5.4％;线性范围达400 ng。     

涂钼石墨管-石墨炉原子吸收法测定人发中的微量铍

比较了多种涂层金属和基体改进剂对石墨炉原子吸收法(GFAAS)测定微量铍的影响,建立了涂钼石墨管硝酸锂作基体改进剂测定铍的新方法,方法灵敏,抗干扰能力强。方法的线性范围为0～20ng/mL,RSD为4.8%(n=10),检出限为1.4×10-10g/mL。用该法测定了土壤标样及人发样品中的铍,结果满意。     

石墨炉原子吸收法直接测定血清中硒,砷

选用Ｐｄ－Ｎｉ－Ｔｒｉｔｏｎ Ｘ－１００为基体改进剂，用石墨炉原子吸收法直接血清中砷、硒。该法具有操作简单、快速、灵敏度高的特点，为临床测定血清中砷、硒提供了一种新方法。     

氢化物发生-原子荧光光谱法测定麦饭石中的硒含量

采用氢化物发生-原子荧光光谱法测定麦饭石中的硒.在优化的实验条件下,标准曲线的线性范围为0～20 ng/mL,相关系数r=0. 9997,检出限为0. 40 ng/mL.测定结果的相对标准偏差为0. 69%(n=11),加标回收率为92. 0%～106. 0%.该方法测定麦饭石中的硒是可行的.     

微波消解样品-石墨炉原子吸收光谱法测定蜂产品中铅、镉、硒

提出了石墨炉原子吸收光谱法测定4种蜂产品中硒、铅和镉的含量.样品用浓硝酸、过氧化氢浸泡后,加热溶解,补加浓硝酸、过氧化氢进行微波消解.在优化的石墨炉工作条件下,用磷酸二氢铵作基体改进剂测定铅和镉,用PdCl2和Mg(NO3)2作混合基体改进剂测定硒.铅、镉和硒的检出限(3S/N)分别为11.3,1.9,3.7 ng,应用此方法分析了4种蜂产品样品,并用标准加入法作回收试验,测得铅、镉、硒的回收率分别为95.4%～103.8%,89.0%～110.0%,86.8%～96.5%之间,相对标准偏差均小于6%.     

流动注射氢化物发生电加热石英管原子吸收光谱法测血清硒

采用自控电热消化器消化血清 ,消化液经流动注射氢化物发生 电加热石英管 原子吸收光谱法测定血清硒。该方法的检出限为 0 .4 5ng·ml- 1,同一血样 8次测定相对标准偏差为 3 59% ,用该法测定了冻干牛血清标准物质和牛血清标准物质 ,测定结果均落在标准物质的不确定度范围内。方法准确、简便、灵敏 ,已用于临床血清硒样本的测定     

石墨炉原子吸收光谱法直接测定生物样品痕量硒

近年研究表进,克山病,大骨节病和动物的白肌病是与硒量低有密切的关系。因此,生物体内痕量硒的测定,引起人们的重视和兴趣。由于硒的挥发性和基体干扰,影响石墨炉原子吸收法直接测定的准确性。基体改进剂的使用,能改善分析灵敏度。Ni(NO_3)_2是最常用的基体改进剂。Wely等提出用Mg(NO_3)_2和Cu(NO_3)_2作混合基体改进剂,可有效地稳定不同价态的Se挥发。本文比较了几种基体改进剂消除干扰的效果,用Ni(NO_3)_2和K_2ptCl_6为混合基体改进剂,直接测定血液和白内障中痕量硒,获得满意的结果。     

流动注射氢化物发生电加热石英管原子吸收光谱测定测血清硒

采用自控电热消器消化血清,消化液经流动注射氢化物发生－电加热石英管－原子吸收光谱法测定血清硒。该方法的检 为0．45mg.ml^-1,同一血样8次测定相对标准偏差为3．59％,用该法测定了冻干牛血清标准物质和牛血清标准物质,测定结果均落在标准物质的不确定度范围内。方法准确、简便,灵敏,已用于临床血清硒样本的测定。     

塞曼石墨炉原子吸收光谱法测定茶叶中镉

建立了石墨炉原子吸收光谱法测定茶叶中镉含量的分析方法。以1%磷酸二氢铵 1%硝酸镁的混合液为基体改进剂测定了茶叶中的镉,方法的回收率96.0%~103.0%,检出限为0.076ng/mL,测定结果令人满意。     

Determination of selenium in human serum by liquid chromatography/electron capture atmospheric pressure chemical ionization mass spectrometry after acid digestion and derivatization using 2,3-diaminonaphthalene

Analysis of selenium in biological samples is very important and numerous analytical methods for the element have been developed. One of the most convenient and widely used methods for routine determination of serum selenium is a fluorometric method using 2,3-diaminonaphthalene (DAN); however, this method lacks specificity. We observed that 4,5-benzopiazselenol (BPS), a selenium derivative of DAN, is ionized with electron capture in an atmospheric pressure chemical ionization (APCI) interface, and subsequently established a method for determining total human serum selenium by means of liquid chromatography/atmospheric pressure chemical ionization mass spectrometry. All pretreatment procedures were carried out in a single test tube to minimize selenium loss. The recovery of organic or inorganic selenium spiked to human serum was 97-103%.The detection limit of BPS was equivalent to 0.2 ng of selenium and the lower quantitative limit of serum selenium was 10 ng mL(-1). The coefficient of variation of standard concentrations in control serum samples was 4.5%. The purity of the observed peak obtained from serum samples was confirmed using the ion cluster technique.     

硒(Ⅳ)-碘化物-结晶紫体系的共振发光和二级散射光谱

硒（Ⅳ）－碘化物－结晶紫体系的共振发光和二级散射光谱刘绍璞,刘忠芳（西南师范大学环境化学研究所,重庆,６３０７１５）关键词共振发光,二级散射,反二级散射,硒（Ⅳ）－碘化物－结晶紫体系,硒的测定长期以来,溶液体系的共振发光和二级散射现象常常被人们忽略。...     

Determination of novobiocin by a kinetic spectrophotometric method in milk and biological samples

A new, simple, inexpensive, and fast kinetic spectrophotometric method was developed for the determination of trace amounts of antibiotic drug novobiocin sodium over the range of 4?32 ng/mL. The method is based on the inhibitory effect of novobiocinon the reaction of Amido Black and periodate in the acidic micellar mediums. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance at 627 nm and fixed-time 6 min from initiation of the reaction. The detection limit is 3 ng/mL, and relative standard deviation for 4.8 and 12 ng/mL novobiocin were 0.52 and 0.65%, respectively, for six replicate measurements. The method was applied to the determination of novobiocin in human and dog serum, urine, and milk samples.     

分子荧光光谱法测定富硒大米中的痕量硒

硒(Ⅳ)与DAN(2,3-二氨基萘)生成具有荧光特性的4,5-苯并苤硒脑,可用分子荧光光谱法测定,优化测定的实验条件,建立了快速准确测定大米中痕量硒的方法.结果表明,其最佳测定条件为:pH=2.0,反应温度为80℃,1.0×10-5 mol/L十六烷基溴化吡啶用作表面活性剂,环己烷萃取条件下,增敏效果明显,在0～0.0...     

荧光动力学法测定痕量硫氰根离子的研究

本文利用痕量硫氰根离子对溴酸钾氧化罗丹明６Ｇ反应的抑制作用，建立了痕量硫氰根离子的荧光动力学检测方法。方法检测限０．４ｎｇ／ｍＬ。线性范围０．４－３２．０ｎｇ／ｍＬ。应用于吸烟人和非吸烟人唾液、湖水、血清中痕量硫氰根离子的测定，结果令人满意。     

Kinetic spectrophotometric determination of trace amounts of selenium and vanadium

A sensitive kinetic spectrophotometric method has been developed for the determination of Se(IV) over the range of 45 to 4000 ng in 10 mL of solution. The method is based on the catalytic effect of Se(IV) on the reduction reaction of bromate by hydrazinium dichloride, with subsequent reaction of Ponceau S with products of the above reaction (chlorine and bromine), causing color changing of Ponceau S. Method development includes optimization of time interval for measurement of slope, pH, reagents concentration, and temperature. The optimized conditions yielded a theoretical detection limit of 33 ng/¶10 mL of solution of Se(IV). The interfering effects were studied and removed. The method was applied to the determination of selenium in spiked water, Kjeldahl tablet, selenium tablet, and shampoo. Vanadium(V) has an inhibition effect on the catalyzed reaction of bromate and hydrazine by selenium. Using this effect, V(V) can be determined in the range of 70 to 2500 ng in 10 mL of solution. The optimization procedure includes pH and selenium concentration. An extraction method was used for interference removal. The method was applied to the determination of vanadium in petroleum.     

Kinetic spectrophotometric determination of trace amounts of selenium and vanadium

A sensitive kinetic spectrophotometric method has been developed for the determination of Se(IV) over the range of 45 to 4000 ng in 10 mL of solution. The method is based on the catalytic effect of Se(IV) on the reduction reaction of bromate by hydrazinium dichloride, with subsequent reaction of Ponceau S with products of the above reaction (chlorine and bromine), causing color changing of Ponceau S. Method development includes optimization of time interval for measurement of slope, pH, reagents concentration, and temperature. The optimized conditions yielded a theoretical detection limit of 33 ng/?10 mL of solution of Se(IV). The interfering effects were studied and removed. The method was applied to the determination of selenium in spiked water, Kjeldahl tablet, selenium tablet, and shampoo. Vanadium(V) has an inhibition effect on the catalyzed reaction of bromate and hydrazine by selenium. Using this effect, V(V) can be determined in the range of 70 to 2500 ng in 10 mL of solution. The optimization procedure includes pH and selenium concentration. An extraction method was used for interference removal. The method was applied to the determination of vanadium in petroleum. Received: 20 October 1998 / Revised: 17 April 1999 / Accepted: 3 June 1999     

[HgI4]2－-蛋白质离子缔合物体系共振瑞利散射和共振非线性散射光谱及其分析应用

在0.0035～0.0045 mol/L硫酸介质中, 牛血清白蛋白(BSA)、人血清白蛋白(HSA)、卵白蛋白(OVA)和血红蛋白(HGB)等蛋白质以带正电荷的阳离子存在. 它们能借助于静电引力和疏水作用力与配阴离子[HgI4]2－-反应形成结合产物, 此时将引起共振瑞利散射(RRS)、二级散射(SOS)和倍频散射(FDS)显著增强, 并且出现新的散射光谱. 其最大RRS, SOS和FDS波长分别位于390, 760和390 nm附近. 在一定范围内, 三种散射增强(ΔIRRS, ΔISOS和ΔIFDS)与蛋白质浓度成正比, 方法具有高灵敏度, 三种方法对于不同蛋白质的检出限分别在5.7～15.9 ng/mL (RRS), 8.2～15.4 ng/mL (SOS)和11.2～22.1 ng/mL (FDS)之间, 均可用于痕量蛋白质的测定. 本文研究了[HgI4]2－与蛋白质相互作用对RRS, SOS和FDS光谱特征和强度的影响, 考察了适宜的反应条件, 并以RRS为例考察了共存物质的影响, 表明方法有良好的选择性. 据此, 利用[HgI4]2－与蛋白质的相互作用发展了一种用共振光散射技术、灵敏度高、简便、快速测定蛋白质的新方法. 本方法可用于血清和人尿中总蛋白质的测定.     

溴酸钾氧化吡口罗红G催化动力学光度法测定痕量NO-2

研究了在磷酸介质中亚硝酸根催化溴酸钾氧化吡口罗红Ｇ而使其褪色，建立了催化动力学光度法测定痕量亚硝酸根的新方法，测定范围为０．２～２０μｇ／ｍＬ，检出限为０．２ｎｇ／ｍＬ，用于食品和水样中的亚硝酸根测定获得满意结果     

Effects of the Interaction of Rifamycin SV with Serum Albumins on the Resonance Rayleigh Scattering Spectra and Their Analytical Application

In pH 4.5–4.8 Britton‐Robinson buffer solution, rifamycin SV (i.e. rifamycin sodium) can react with serum albumin such as human serum albumin (HSA) and bovine serum albumin (BSA) to form macromolecular complexes by electrostatic attraction and hydrophobic force. As a result, the resonance Rayleigh scattering (RRS) of the drug was enhanced remarkably and the RRS peaks were at 374 and 552 nm. The enhancement of RRS (ΔI) is directly proportional to the concentration of HSA or BSA. The linear ranges and the detection limits are 0.03–6.0 µg/mL and 9.0 ng/mL for HSA, and 0.01–8.0 µg/mL and 2.0 ng/mL for BSA, respectively. In this work, a sensitive, selective, simple and fast method for the determination of trace amounts of serum albumin by RRS technique has been developed, which was applied to the determination of serum albumin in the synthesized samples and human urine samples with satisfactory results.