微波消解——冷原子只收法定量测定人参中汞的研究

应用微波消解仪的原子吸收光谱仪,采用氢化物－冷原子吸收光谱法对人参中的汞的定量测定方法进行了研究。对微波消解仪的消解条件、氢化物－冷原子吸收方法的测定条件进行了探讨。在本法选择的条件下,回收率为90．98％－108．96％,相对标准偏差为8．04％－15．77％。与国家标准方法的对比实验证明,两者无显著差异。     

微波消解-冷原子吸收法定量测定人参中汞的研究

应用微波消解仪和原子吸收光谱仪,采用氢化物－冷原子吸收光谱法对人参中的汞的定量测定方法进行了研究和探讨。对微波消解仪的消解条件、氢化物－冷原子吸收法的测定条件进行了探讨。在本文选择的条件下,回收率为90．98％－108．96％,相对标准偏差为8．04％－15．77％。与国家标准方法的对比实验无显著差异。     

控温消解-冷原子吸收方法测定水果蔬菜中微量汞

应用程序控温－湿法消解－氢化物发生－冷原子吸收光谱法对水果蔬菜中的汞的定量方法进行了研究和探讨。对程序控温消解仪的消解条件、氢化物－冷原子吸收的测定条件进行了探讨。在本文选择的条件下，回收率为86．99％－108．00％，相对偏差为4．6％－10．8％。该方法与国家标准方法相对照，无明显差异。     

微波消解-火焰原子吸收法测定土壤中的钴

建立了微波消解一火焰原子吸收法测定土壤中钴的方法：用微波消解土壤、电热板加热驱酸的方法对土壤样品进行前处理,优化了微波消解条件。方法的加标回收率为93．0％～106．0％,检出限为3．0μg/g,测定结果的相对标准偏差为2．1％～4．9％（n=6）。     

微波消解样品-冷原子吸收光谱法测定鱼粉中微量汞

以微波溶样技术消解样品,采用正交试验设计优化冷原子吸收光谱法测定汞的试验条件,并对微波消解条件和共存离子的干扰进行了试验。试验表明：汞含量在30μg·L^-1范围内服从比耳定律,方法的检出限为0．13μg·L^-1,相对标准偏差为2．6％,回收率为97．6％～106．8％。     

电感耦合等离子体原子发射光谱法测定动物源抗癌中药中痕量铅

以微波消解样品,在碱性铁氰化钾溶液中进行铅的氢化物发生反应.采用连续氢化物发生器,对电感耦合等离子体原子发射光谱法测定痕量铅的条件进行了研究,方法的检出限(3σ)为0.72μg·L-1,相对标准偏差(n=11)为1.22%,应用于动物源抗癌中药中痕量铅的测定,回收率在96.6%～100.1%之间.     

微波消解氢化物发生ICP—AES法测定川山紫中痕量硒

建立了微波消解连续氢化物发生ICP AES法测定川山紫中痕量硒的方法 ,系统地研究了微波消解、氢化物发生的最佳条件 ,方法简便快速 ,检出限为 0 .0 0 38μg·ml- 1,RSD为 1.13% (n =10 ,0 .5 4 7μg·g- 1Se) ,样品加标回收率为 99.2 4 %。     

微波消解-氢化物发生-原子荧光光谱法测定出口芳香油中痕量铅

采用微波消解技术溶样,氢化物发生-原子荧光光谱法测定了出口芳香油中痕量铅.系统地研究了微波消解、氢化物发生的最佳条件,方法简便快速,在选定的实验条件下,方法检出限为0.25 μg·L~(-1),相对标准偏差小于5%,回收率为86.5%～100.5%.     

微波消解-原子吸收光谱法间接测定垃圾中的硫含量

建立了用微波消解技术处理样品,原子吸收光谱法间接测定城市生活垃圾中硫含量的分析方法。优化了微波消解及原子吸收仪器的最佳操作条件。方法可用于城市生活垃圾中硫的测定,相对标准偏差小于2.5%,回收率为95.3%～101.7%。     

超级微波消解-石墨炉原子吸收光谱法测定不同类型土壤中的镉

目的 探讨并建立超级微波消解-石墨炉原子吸收法测定不同类型土壤镉含量的方法。方法 采用超级微波消解仪对样品进行前处理,对比不同消解体系的消解效果,选择合适的的消解体系,采用石墨炉原子吸收法测定镉浓度,同时优化基体改进剂、灰化温度等工作参数,确定最佳的分析条件。结果 在最优方法条件下,标准曲线在0.0～1.0 μg/L浓度范围内线性关系良好,相关系数γ=0.999,检出限浓度为0.04 μg/L,定量限浓度为0.12 μg/L,方法准确度为94.5%～109.8%,精密度为0.6%～5.4%,方法应用于不同类型土壤标准物质镉的测定,测得结果均在标准值范围内。结论 本方法方便快捷、准确高效、用酸量低、节约环保,便于在基层推广,适用于批量不同类型土壤样品镉的污染监测工作。     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

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.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

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.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

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.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

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%).     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.     

Synthesis of N-substituted carbazolones from α-iodo enaminones via Pd(0)-catalyzed intramolecular coupling under microwave irradiation

A variety of N-aryl and N-alkyl carbazolones were conveniently achieved in good to high yields via Pd₂(dba)₃-mediated intramolecular coupling of N-substituted α-iodo enaminones under microwave irradiation. The Pd(0)-catalyzed cyclization was found to proceed favorably with the more electron-deficient phenyl ring during the reactions involving unsymmetrical N,N-diaryl α-iodo enaminones. This unique property enables the construction of carbazolone skeleton containing nitro substituted benzenoid ring.     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of substituted 2,4,5,6-tetrahydrocyclopenta[c]pyrazoles and 2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazoles by intramolecular nitrilimine cycloaddition

Both substituted 2,4,5,6-tetrahydrocyclopenta[c]pyrazoles and 2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazoles have been synthesized by the 3+2 intramolecular dipolar cycloaddition of nitrilimines to alkynes. This cyclization has been extended to more versatile 3-bromo derivatives by the use of alkynylbromides as dipolarophiles.