液相色谱法测定鳗鱼中的孔雀石绿

用高效液相色谱法测定鳗鱼组织中孔雀石绿的残留量。鱼体中残留的孔雀石绿在酸性介质下，经高速均质后，用乙腈均质提取，合并提取液，用二氯甲烷再次萃取，有机相过无水硫酸钠和氧化铝复合小柱后浓缩至干，用盐酸羟胺和流动相定容。以乙酸盐缓冲溶液和乙腈为流动相，在KR60－5氰柱上分离后，用可见光检测器在618nm处测定吸光强度，外标法定量。其检出限为1μg/kg，回收率为93.5%-99.6%，相对标准偏差RSD为6.54%-11.0%。     

火焰原子吸收分光光度法测定复合肥料中的钾含量

以K404.4nm作为分析线，研究了火焰原子吸收分光光度法测定复合肥料中钾含量的方法。该方法的线性范围为0－208mg/L，线性回归方程为A＝0.0026c-0.0100，相关系数r=0.9992，RSD为2.4%-5.0%，回收率为95.6%-101.3%。该方法的测定结果与四苯硼酸钾重量法基本一致，且方法简便、快速。     

火焰原子吸收分光光度法测定饲料中的钙含量

采用硝酸锶作干扰制剂，不经分离，直接用火焰原子吸收分光光度法测定饲料中的钙含量。该方法的线性范围为0-7.0μg/ml。线性回归方程为A=37.5169C 1.1143，相关系数r=0.9998，相对标准偏差为0.59%-1.53%，回收率为98%-100.5%。该方法简便、快速。     

薄层色谱-紫外分光光度法测定 溴敌隆乳油中的有效成份

用薄层色谱－紫外分光光度法分离和测定溴敌隆乳油中的有效成份,样品以甲醇－乙酸乙酯－石油醚（10：20：8）为展开剂在硅胶G板上展开,在波长262nm处测定分析,方法在0.25－1.50mg/mL范围内有良好的线性关系,检出限为0.08mg/mL,RSD值为1.9%(n=10),回收率97.1%-102.1%。     

石墨炉原子吸收光谱法测定岩石中的镓、铟、锗

建立了测定岩石中镓、铟、锗的石墨炉原子吸收光谱法。镓、铟、锗的线性范围分别为0-50、0－5、0－20μg/mL，线性相关系数分别为0.996、0.935、0.992，回收率分别为97.3%-108.0%、95.0%-105.0%、93.3%-102.0%，相对标准偏差分别为3.6%、13.3%、8.7%，检出限分别为0.042、0.001、0.008μg/mL。     

高效液相色谱法测定滇白珠植物中滇白珠甙

提出反相高效液相色谱法测定滇白珠甙含量的方法。反相Kromasil C18柱，甲醇－乙腈－水（V／V）＝25：5：70为流动相，紫外220nm检测，外标法定量。线性范围为0.005-0.800g/L，r=0.9997-0.999，方法回收率和标准偏差分别在98.605-102.90%和0.58%-0.69%之间（n=6），3种甙的检测限在0.01-0.02mg/L之间。本方法快速、准确、重现性好，适用于工艺生产中质量控制。     

协同催化——溶剂萃取光率法测定血清中的唾液酸

利用Cu^2 和Cr^3 的协同催化作用,促进间苯二酚与唾液酸的显色,再用乙酸丁酯——正丁醇萃取有色物质,变换波长至625nm处测定;血清中的唾液酸含量。建立了血清中唾液酸测定的新方法,方法的线性范围为0－1000mg/L,检出限为2.1mg/L,相对标准偏差为1.59%-2.11%,回收率为96.2%-101.2%,糖类及抗坏血酸等物质对测定的干扰＜2％。该法简单、快速、灵敏、准确,可用于临床体液中唾液酸的测定。     

高效液相色谱法测定保健食品中的黄芪甲甙

以Waters Nova-Pak C18柱为色谱柱，乙腈－水（体系比为1：2）为流动相，Waters-2996二极管阵列检测器为检测器，对保健食品中的黄芪甲甙进行高效液相色谱分析。线性回归方程为A＝89852c-22076，相关系数r=0。9997,线性范围为5.0-50.0μg/mL，回收率为97.2%-98.9%，相对标准偏差为1.38%-1.61%。方法简便，灵敏度高，重现性好。     

高效溶剂萃取－固相萃取/气相色谱－质谱法测定大气颗粒物中多环芳烃和有机磷阻燃剂

建立了高效溶剂萃取（HPSE）－固相萃取（SPE）/气相色谱－质谱（GC－MS）测定大气颗粒物中16种多环芳烃（PAHs）和15种有机磷阻燃剂（OPFRs）的方法。以正己烷－二氯甲烷（1∶1,体积比）溶液为萃取溶剂,萃取液旋转蒸发浓缩后经Florisil固相萃取柱净化,PAHs和OPFRs的洗脱溶剂分别为10 mL正己烷－二氯甲烷（1∶1）和10 mL乙酸乙酯,洗脱液浓缩定容后进行GC－MS测定。16种PAHs和15种OPFRs的线性范围为0.001 ~ 2.0 μg/mL,相关系数（r2）均大于0.99;检出限（LOD,S/N = 3）分别为0.10 ~ 10.00 μg/L和2.59 ~ 75.00 μg/L,定量下限（LOQ,S/N = 10）分别为0.33 ~ 33.33 μg/L和8.63 ~ 250.00 μg/L;平均回收率分别为73.0% ~ 98.0%和69.3% ~ 111%,相对标准偏差（RSD）分别为3.7% ~ 13%和2.5% ~ 17%。该方法适用于大气颗粒物样品中多环芳烃和有机磷阻燃剂的测定。     

ICP-AES测定废Al2O3基催化剂中Pt、Pd

研究了废Al2O3基催化剂中Pt,Pd的ICP－AES测定新方法。以王水溶解样品，在HCl(5 95)介质中，用工作曲线法对废Al2O3基催化剂中的Pt,Pd直接进行测定，不需进行基体匹配。方法的检出限分别为：Pt 0.1μg/mL，P 0.045μg／mL；样品的加标回收率为Pt 95.2%-105.5%,Pd 95.3%-100.6%;RSD(n=6)均＜9％。     

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%).     

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.     

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.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

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.