钙制剂中铝含量分析方法

钙制剂中铝含量分析方法,涉及一种化学分析方法,该方法为荧光分光光度法测定钙制剂中铝的含量,包括以下荧光分析条件和样品处理两个步骤:(1)荧光分析条件为:激发波长,发射波长,狭缝宽度,灵敏度;(2)样品处理:络合提取,萃取;将钙制剂移至分液漏斗中,加入8-羟基喹啉、三氯甲烷溶液萃取3次;合并萃取液,置于容量瓶中,加入三氯甲烷定容至标线,摇匀,记录荧光强度;其激发波长Ex=392nm,狭缝宽10 nm,发射波长Em=518 nm,狭缝宽20 nm,灵敏度为2。本发明为测量钙制剂中铝含量提供了一种有效可靠的分析方法。     

铝(Ⅲ)-氧氟沙星-十二烷基硫酸钠荧光体系测定微量铝的研究

在NaAc HAc介质中,溶液中的铝(Ⅲ)能与氧氟沙星和十二烷基硫酸钠(SDS)反应生成一稳定的络合物,使氧氟沙星的内源性荧光显著增强,据此建立了铝(Ⅲ) 氧氟沙星 SDS体系测定铝(Ⅲ)的荧光分析新方法。该体系的最大激发波长λex=365nm,最大发射波长λem=480nm,铝(Ⅲ)浓度在2.0×10-7～5.0×10-5mol L范围内,与荧光增强程度成正比。该方法可直接用于水样和食品中微量铝(Ⅲ)的测定。     

钙制剂中铝含量分析方法等

申请公布号：CN104359881A 申请公布日：2015.02.18申请人：沈阳化工大学
　　摘要钙制剂中铝含量分析方法,涉及一种化学分析方法,该方法为荧光分光光度法测定钙制剂中铝的含量,包括以下荧光分析条件和样品处理两个步骤：（1）荧光分析条件为：激发波长,发射波长,狭缝宽度,灵敏度;（2）样品处理：络合提取,萃取;将钙制剂移至分液漏斗中,加入8-羟基喹啉、三氯甲烷溶液萃取3次;合并萃取液,置于容量瓶中,加入三氯甲烷定容至标线,摇匀,记录荧光强度;其激发波长Ex=392nm,狭缝宽10 nm,发射波长Em=518 nm,狭缝宽20 nm,灵敏度为2。本发明为测量钙制剂中铝含量提供了一种有效可靠的分析方法。     

铝试剂的荧光光谱与荧光量子产率

首次研究了铝试剂的荧光光谱和荧光量子产率,发现pH3至pH12条件下,用紫外光照射铝试剂溶液可以产生荧光,最大激发波长和最大发射波长分别为297nm和409nm,荧光强度与铝试剂浓度之间存在良好的线性关系,线性范围为0.01～3μg/mL,检测下限为0.01μg/mL,以硫酸奎宁为参比,测得铝试剂的荧光量子产率为0.16。     

吡哆醛异烟酰腙与铝荧光反应的研究

合成了新荧光试剂吡哆醛异烟酰腙,研究了该试剂与铝的荧光反应体系,反应在pH4.85水溶液介质中进行,络合物的荧光激发波长λ_(ex)=410nm;发射波长λ_(em)=453nm。铝量在0～0.8μg/10ml范围内,荧光强度与铝量成正比,方法灵敏度为0.2ng/ml。络合物组成比1:1。实验了28种离子存在下的干扰情况。方法直接应用于化学试剂中痕量铝的测定,精密度好,结果令人满意。     

CdTe量子点荧光光度法测定诺氟沙星的含量

在水溶液中合成了巯基乙酸修饰的CdTe量子点,基于铝敏化喹诺酮类抗生素,研究了诺氟沙星与CdTe量子点的荧光增敏作用,建立了用CdTe量子点作为荧光探针检测微量诺氟沙星的新方法。该体系的最大激发波长λex=365nm,最大发射波长λem=586nm。诺氟沙星溶液的浓度在9×10-3～2.4μg·mL-1范围内与体系荧光强度呈良好的线性关系,检出限为4.5×10-3μg·mL-1,相对标准偏差为0.9%。本方法灵敏度较高,选择性较好的,可用于药物中诺氟沙星含量的测定,结果较为满意。     

水中痕量铝离子的浊点萃取-荧光光度法测定

建立了荧光光度法测定水中痕量铝离子的浊点萃取分离富集新体系.在pH 6.0的HAc-NaAc缓冲体系中,水样中的铝与8-羟基喹啉生成疏水性络合物.通过85 ℃水浴加热40 min,8-羟基喹啉-铝络合物被萃取到Triton X-100表面活性剂相并与水相分开.将表面活性剂相用乙醇分散稀释至2.0 mL,在激发波长375 nm和发射波长510 nm下进行荧光测定.测定铝的线性范围为4.0 ～200.0 μg/L,方法的检出限为1.2 μg/L,相对标准偏差(RSD)为4.5%(n=11).方法用于自来水、矿泉水、河水和湖水中痕量铝的测定,加标回收率为92% ～108%.     

CaWO4荧光体的微波热法合成和光致发光

本文报道微波热法合成 Ca WO4荧光体 ,X射线粉末衍射分析确证为四方晶系 ,Ca WO4:Pb0 .0 1 荧光体最大激发波长 λex=2 66.0 nm,最大发射波长 λem=450 .0 nm,在 2 54nm激发下 ,色坐标 x=0 .1 66,y=0 .1 2 4 ,与市售同类荧光体比较 ,相对发光亮度 86% ,荧光体中心粒径 D50 为9.1 8μm,体积比表面 SV 为 81 93 1 / cm。     

水杨基萤光酮-溴化十六烷基三甲铵荧光猝灭法测定微量铝的研究

近几年,用各种新型试剂荧光光度法测定铝的文献报道颇多,其原理多采用铝与某一荧光试剂生成产生荧光的配合物进行测定。但利用铝(Al)-水杨基萤光酮(SAF)-溴化十六烷基三甲铵(CTMAB)三元配合物的形成,使试剂(SAF-CTMAB)荧光猝灭而测定铝的方法尚未见报道。笔者发现,在汞弧光激发下,SAF产生波长为515nm的较强荧光,引入     

同步荧光光谱法测定人体尿液中加替沙星

研究了尿样中加替沙星在不同酸碱条件下的荧光特性,发现在中性水溶液中加替沙星的荧光较弱,荧光发射峰位于450 nm,尿样背景荧光发射峰位于370 nm。由于加替沙星与尿样背景荧光的发射波长部分的重叠,尿样中的加替沙星采用通常的荧光光谱法无法测定。当pH=4.1时,加替沙星的荧光发射显著增强,荧光发射波长由450 nm红移至478 nm,同时尿样背景荧光反而由中性水溶液中的370 nm紫移到355nm。据此建立了一种无需分离直接测定尿样中加替沙星的同步荧光光谱新方法。选择△λ=90 nm,在优化条件下,测定加替沙星的线性范围为0.12~3.2μg.mL-1,检出限为0.04μg.mL-1。方法用于尿样中加替沙星含量的测定,其回收率为92.6%~96.8%,相对标准偏差为1.6%~2.4%。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.