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1.
单扫描极谱法连续测定人发中的微量元素锌铁锰铜   总被引:3,自引:0,他引:3  
本提出在0.15mol/L乙二胺-7.5×10^-3mol/L三乙醇胺-2.5×10^-2mol/L硫氰酸钾底液中单扫描极谱法测定锌、铁、锰,续加硫酸(0.3mol/L)测定铜的方法,峰电位分别为-1.42V,-1.63V,-1.71V,-0.48V(vs.SCE),线性范围:0.05~1.4μg/mLMn,0.04~1μg/mLCu,最低检出浓度.03,0.05,0.02,0.04μg/mLM  相似文献   

2.
倒数示波计时电位法同时测定粮食中Cu、Pb含量   总被引:1,自引:0,他引:1  
在分别含有2g/L乙二胺与*10^-4mol/L8-羟基喹啉(Oxine)和0.3mol/L的氢氧化钠淀粉液中,Cu^2+、Pb^2+具有良好的示波图。其切口电位分别为-0.85V,-120V(vs.SCE),二者相差0.35V,能够分辨,可同时测定,本方法应用于大米中Cu、Pb含量的同时测定,检出限分别为5.8μg/L(Cu)、10.0μg/L(Pb),平均回收率为96.0%、102.0%。  相似文献   

3.
依诺沙星在混合粘合剂碳糊电极上的电化学特性   总被引:5,自引:2,他引:3  
制备了混合粘合剂碳糊电极。在0.015mol/L,磷酸-0.10mol/LKCl溶液中,依诺沙星在该电极上于-1.26V处产生一灵敏的阴极溶出伏安峰。在-0.90V富集90s后,依诺沙星的线性范围为3.1×10^-7-1.2×10^-5mol/L,检测下限为9.42×10^-8mol/L,所提出的方法用于尿液和血清中依诺沙星测定,回收率在96%-103%之间。  相似文献   

4.
反相高效液相色谱分离—安培法检测酚类化合物   总被引:4,自引:0,他引:4  
辛梅华  徐金瑞 《分析化学》1994,22(5):505-508
本文报道了RP-HPLC-安培法检测测定酚类化合物的条件,在Shim-packCLC-C8柱上用含0.5mol/L NaH2PO4缓冲溶液的5%甲醇水溶液洗脱分离,于E+1.0V处检测,线性范围在0-7μg/ml,检测限达ng/ml。  相似文献   

5.
丁基罗丹明B—钼酸盐光度法连续测定铈和钪   总被引:4,自引:0,他引:4  
王加林  徐其亨 《分析化学》1996,24(3):344-347
在聚乙烯醇(PVA)存在下,丁基罗丹明B(BRB)分别与铈钼、钪钼杂多酸络阴离子形成离子缔合物,其最大吸收均位于570nm,表面摩尔吸光度分别为εCe=3.96×10^6L.mol^-1.cm^-1,εSc=4.71×10^5L.mol^-1.cm^-1,服从比耳定律范围分别为0-24μg/L Ce和0-60μg/LSc,测定极限为Ce1.0μg/L(n=12)和Sc1.9μg/L(n=10),对  相似文献   

6.
二阶导数差示脉冲极谱法用于醋酸氟氢可的松的定量研究   总被引:2,自引:0,他引:2  
用二阶导数差示脉冲极谱法对醋酸氟氢可的松进行了定量分析。在0.001mol/L硫酸+乙醇+水(1+25+24)的底液中,醋酸氟氢可的松于-0.340V(vsAg/AgCl)处出现一良好的二阶导数差示脉冲极谱峰,在5~140μg/mL范围内,醋酸氟氢可的松的浓度与其二阶导数差示脉冲极谱峰幅值呈线性关系,检测限为0.4ng/mL。本法操作简便、快速、灵敏、结果准确。  相似文献   

7.
以1-(2-噻唑偶氮)-2-萘酚(TAN)作柱前显色剂,于ODS柱上,用内含0.1mol/LLiCl,5×10-6mol/L TAN和HAc-NH4Ac缓冲溶液(pH 5.5)的甲醇-水溶液(80:20,V/V)作流动相,流速为0.6mL/min,并以紫外-可见检测器于590nm处进行检测,发展了一种RP-HPLC法同时分离测定铜(Ⅱ)、铁(Ⅱ)、镍(Ⅱ)的方法,方法灵敏度高,对于铜、铁、镍的检测限分别为1μg/L, 2 μg/L和 0.4 μg/L。用于实际样品测定,结果满意。  相似文献   

8.
本实验运用一阶导数差示脉冲极谱法对甲硝唑及其制剂进行了定量研究。在0.001mol/L氯化钾-0.001mol/L盐酸-水(1+0.2+48)的底液中,甲硝唑于-0.800V(vs Ag/AgCl)处出现一良好的一阶导数差示脉冲极谱峰,在50~300μg/mL范围内,药物浓度与其导数峰幅值呈线关系,检测限为8.0×10^-8mol/L。本法操作简便,快速,灵敏,结果准确。  相似文献   

9.
铽-环丙沙星体系的荧光特性及环丙沙星的测定   总被引:17,自引:0,他引:17  
近中性条件下,铽(Ⅲ)能与环丙沙星(ciprofloxacin)反应形成1:2的络合物。利用这一反应,建立了简单、快速、灵敏的测定环丙沙星的荧光方法,并且详细讨论了测定的各种条件。测定的最佳条件为:λex/λem=325.0/545/0nm,Tb^3+(3.0*10-3mol/L)2.0mL,pH=6.0的NaAc-HAc缓冲溶液2.0mL。线性范围13-1000μg/L,回归方程为F=5.42+0.2207μg/L)(r=0.998);检出限为10μg/L。此方法用于血清及环丙沙星片剂的测定,结果令人满意。  相似文献   

10.
在醋酸-醋酸钠缓冲溶液中,钛与苯甲酰苯基羟胺形成的络合物,在示波极谱仪上产生-灵敏的吸附波,导数峰电位E_p=-0.83V(vs.SCE),检出限0.1μg/L,线性范围0~5μg/L.选择性较好,本法已用于测定高铝水泥标样中的钛。  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.
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   

16.
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   

17.
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   

18.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

19.
20.
N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).  相似文献   

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