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1.
桑色素荧光光度法测定二氯化双(丁氧羰乙基)锡   总被引:1,自引:1,他引:0  
在pH3.0的HAc-NaAc缓冲溶液中和有Triton X-100存在下,二氯化双(丁氧羰乙基)锡(简写为R2SnCl2)与桑色素形成1:1的荧光络合物。络合物的激发波长和发射波长分别为443.2nm和514。4nm。R2SnCl2中的Sn浓度在0 ̄3.0mg/L范围内,与络合物荧光强度呈线性关系。方法检出限为7.81μg/L Sn,用于PVC中间产品和污水中R2SnCl2的测定,结果满意,相对  相似文献   

2.
分光光度法研究血清蛋白质与钍试剂Ⅰ的作用   总被引:10,自引:0,他引:10  
钍试剂Ⅰ是测定无机离子的显色剂,在pH 3.8 的Britton-Robinson缓冲溶液中,该试剂能与血清蛋白质形成复合物,λm ax为535 nm ,比试剂本身红移约55 nm ,表观摩尔吸光系数为3.56 ×105 L·m ol- 1·cm - 1(BSA),测定蛋白质的线性范围,为20~160 m g/L。用于人血清样品总蛋白的测定,RSD为1.05 % (n= 4),回收率约为100 % 。方法基本无干扰。  相似文献   

3.
火焰原子吸收光谱法间接测定非金属材料中氯   总被引:9,自引:0,他引:9  
报道了火焰原子吸收光谱法(FAAS)间接测定非金属材料中氯的方法,采用AgCl沉淀,测定剩余Ag~+间接求出氯含量。方法的特征浓度为0.014mg/L(1%吸收),检出限为0.032mg/L(3),测定下限为0.11mg/L,相对标准偏差(RSD)为1.5%~10%,样品加标准回收率在91.4%-105%之间。  相似文献   

4.
DBSAQ的合成及荧光光度法测定粮食中痕量铝(Ⅲ)的研究   总被引:9,自引:0,他引:9  
报道了新席夫碱试剂3,5-二溴水杨醛缩-8-氨基喹啉(DBSAQ)的合成,用元素分析,红外光谱法测定了其结构,测定了DBSAQ的配度常数,在pH4.00~5.50范围内DBSAQ与Al⒓)形成稳定的荧光配合物,且在λex/λem=430nm/535nm处产生强烈的荧光,其荧光强度与Al(Ⅲ)的浓度在1.2~240ug/L范围内呈线性关系,检出下限为1.2ug/L,并考察了共存离子的影响,选择性高,  相似文献   

5.
HPLC法测定中成药制剂中10-羟基-2-癸烯酸的含量   总被引:6,自引:0,他引:6  
杨江丰  陈理 《色谱》1998,16(2):178-179
 采用SpherisorbC18柱,以甲醇∶水∶磷酸(45∶65∶0.5)为流动相,以UV210nm为检测波长,测定中成药制剂中10-羟基-2-癸烯酸(10-HDA)的含量,10-HDA浓度在0.006~0.030g/L范围内线性关系良好(r=0.9999,n=5),检测限为0.2mg/L(S/N=3∶1)。方法具有定量准确、快速及主峰和杂质分离度高等特点。  相似文献   

6.
过硫酸钾存在下人血清白蛋白的极谱平行催化氢波及其应用   总被引:10,自引:0,他引:10  
报道 K2S2O8存在下人血清白蛋白(HSA)的极谱平行催化氢波。在 0.4 mol/L NH3-NH4Cl(pH 8.58)-0.01 mol/L K2s2O8支持电解质中,HSA产生一个平行催化氢波,峰电位为-1.85 V(vsAg/AgCl)。该平行催化氢波二阶导数峰电流与 HSA浓度在 2.6 × 10-9~9.6 × 10-9mol/L范围呈线性关系。用于人血清样和尿样中HSA的测定,结果满意。  相似文献   

7.
高效液相色谱法测定人血清中头孢克罗   总被引:1,自引:0,他引:1  
 建立了测定人血清中头孢克罗的高效液相色谱法。分析柱为Shim-packCLC-ODS(5μm),6.0mm×150mm;流动相为磷酸盐缓冲液(pH5.8)∶乙腈=87.5∶12.5,流速为1.2mL/min;紫外检测波长为254nm。血清中头孢克罗浓度在0.125~24mg/L范围内,峰高与浓度呈良好的线性关系,回归方程为H=-3.200+92.29C(n=9,r=0.9999),日内、日间变异系数分别为4.1%和5.8%,平均回收率为99.3%。  相似文献   

8.
钍钼杂多酸-丁基罗丹明B测定岩矿中痕量钍   总被引:2,自引:0,他引:2  
本文报道了一个灵敏度高、选择性好的测定痕量钍的新光度分析法。在聚乙烯醇(PVA)存在下,钍钼杂多酸和丁基罗丹明B(BRB)形成离子缔合物,其适宜条件为cHClO4=1.3mol/L,cMoO42-=6.8×10-4mol/L,cBRB=2.7×10-5mol/L,PVA0.08%。络合物的最大吸收波长为570nm,服从比耳定律范围0~0.8mg/25LTh,表观摩尔吸光度ε为3.63×106L·mol-1·cm-1,测定极限1.8μg/L(n=12),对0.02mg/LTh分析11次的相对标准偏差为2.9%,络合物的摩尔组成Th∶Mo∶BRB=1∶12∶7。大多数常见元素、100倍Ce(Ⅲ)、40倍U(Ⅵ)和20倍P(Ⅴ)不干扰钍的测定。本法已用于地质标样中钍的测定,结果满意。  相似文献   

9.
用HPLC/ECD法测定血小板5-HT,运用 WatersμBondapak C柱,3,4二羟基苄胺(DH-BA)作内标,以 0.07 mol/L乙酸钠缓冲液+乙腈为流动相(20+1),每1L缓冲液含 0.05 mol/L柠檬酸、2.5 mmol/L庚烷磺酸钠、0.1mmol/L Na_2EDTA,流速0.8 mL/min。DHBA和 5-HT的保留时间分别为5.4和11.5 min,线性范围为0.025~1mg/L(r= 0.9997)。5-HT日内 RSD低于1.87%,日间RSD低于8.54%,方法回收率为100.4%±2.3%。提示本方法快速简便,灵敏准确,适用于临床基础研究。  相似文献   

10.
高碘酸盐氧化亚甲蓝动力学光度法测定痕量锇   总被引:7,自引:0,他引:7  
以Os(Ⅳ)催化高碘酸盐氧化亚甲蓝(MB)反应为基础提出了测定痕量锇的方法。在90℃加热14min和660nm波长处采用固定时间法测定亚甲蓝吸收的降低,锇浓度在0~3.2μg/L范围呈线性关系,检了限为0.02μg/L,对1.6μg/L Os(Ⅳ)测定的RSD为1.56%(n=11),催化反应对Os(Ⅳ)、MB、KIO4和H2SO4均为一级反应,催化反应的表观活化能为87.72KJ/mol,探讨了  相似文献   

11.
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.  相似文献   

12.
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.  相似文献   

13.
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.  相似文献   

14.
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.  相似文献   

15.
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.  相似文献   

16.
17.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

18.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

19.
Quercetin, the polyphenolic compound, which has the highest daily intake, is well known for its protective effects against aging diseases and has received a lot of attention for this reason. Both quercetin 3-O-β-d-glucuronide and quercetin 3′-O-β-d-glucuronide are human metabolites, which, together with their regioisomers, are required for biological as well as physical chemistry studies. We present here a novel synthetic route based on the sequential and selective protections of the hydroxyl functions of quercetin allowing selective glycosylation, followed by TEMPO-mediated oxidation to the glucuronide. This methodology enabled us to synthesize the five O-β-d-glucosides and four O-β-d-glucuronides of quercetin, including the major human metabolite, quercetin 3-O-β-d-glucuronide.  相似文献   

20.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
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.  相似文献   

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