电感耦合等离子体质谱(ICP-MS)法测定转基因大豆中的无机元素

建立了用电感耦合等离子体质谱(ICP-MS)法测定转基因大豆中无机元素含量的方法,采用浓HNO3溶解转基因大豆,实验结果表明,转基因大豆中Ca、Na、K、Mg、Zn、Fe的含量比较丰富。方法灵敏可靠,测定相对标准偏差(RSD,n=6)均小于3%,方法的加标回收率在97.6%~103%,实验结果为探讨转基因大豆对人体的营养保健作用提供了参考。     

石墨炉原子吸收光谱法测定转基因棉籽中的铅镉铜铬

本文探讨了干法灰化与湿法消解-石墨炉原子吸收光谱法测定转基因与非转基因棉籽中重金属元素铅、镉、铜和铬的方法,比较了两种预处理方法对测定结果的影响.结果表明:两种方法均能满足分析测定的需要.将分析方法应用于转基因与非转基因棉籽中四种重金属含量的测定,结果显示,转基因棉籽中铅和铜的含量明显低于非转基因棉籽,镉和铬的含量与非转基因棉籽相当.     

龙葵Atrazine抗性基因向大豆叶绿体的转移及在转基因植株中的表达

本文将龙葵Atrazine抗性psbA基因采用合子期子房微注射法,导入对Atrazine敏感的大豆叶绿体基因组中,经直接用Atrazine涂抹叶片及叶片在较强光诱导下荧光动力学研究和间接分子杂交试验等检测方法鉴定,表明本项研究首次获得了转基因大豆植株。     

铂纳米颗粒修饰电化学DNA传感器检测大豆中转基因成分

用电沉积方法将铂纳米颗粒修饰在玻碳电极表面,然后将花椰菜花叶病毒35S启动子ssDNA片段直接吸附在铂纳米颗粒上,制成特异的电化学DNA传感器。用扫描电子显微镜和循环伏安法对修饰铂纳米颗粒电极进行了表征。ssDNA探针与互补目的ssDNA杂交,以[Co(phen)3]3 (phen=1,10-Phe-nanthroline)为杂交指示剂,用方波伏安法进行检测,表现出良好的响应信号。与在裸玻碳电极上修饰的探针相比,测定目的基因的灵敏度显著提高。传感器对互补目的ssDNA检测的线性范围为2.14×10-9～2.14×10-7mol/L;检出限为1.0×10-9mol/L,与3个碱基错配的DNA序列杂交,观察不到明显的杂交信号。样品DNA经HindⅢ非限制性内切酶酶切后测定,杂交检测信号增大。用传感器检测含量不同的转基因大豆DNA和非转基因大豆DNA的混合溶液,杂交前后的电流差与转基因DNA的含量呈良好线性关系。连续5次测量含有100%转基因大豆DNA杂交后的电信号,相对标准偏差为5.89%,固定探针的电极再生后可重复使用8次。     

大豆残渣中大豆皂苷含量的分析方法

采用紫外分光光度法测定豆粕残渣中大豆皂苷的含量,结果表明,豆粕残渣中含大豆皂苷,平均回收率94.40%。此方法较准确、简便、重现性好,适用于大豆皂苷产品的质量控制,为大豆残渣的开发利用提供了依据。     

磷酸盐缓冲体系中大豆卵磷脂的分析

建立了一种测定磷酸盐缓冲体系中大豆卵磷脂含量的方法。利用无水乙醇－石油醚（６０～９０℃）萃取剂从磷酸盐缓冲溶液中分离出大豆卵磷脂，再用钼蓝法对大豆卵磷脂含量进行测定。该方法操作简便，定量准确，重现性好，用于胰岛素口腔喷剂中大豆卵磷脂含量测定，样品平均回收率为９９．７５％，ＲＳＤ＝３．９３％。     

国际实验室间转基因产品检测能力验证的研究

以转基因大豆为例，介绍开展APLAC T034国际间实验室转基因检测能力验证的项目。对于样品量值(添加值)的设定进行试验，对样品的均匀性和稳定性进行检验，并对参试实验室的测试结果进行系统的评价和分析。影响转基因产品测试结果的关键因素是检测方法、基因组DNA提取的质量、PCR反应体系中模板DNA的加入量．以及是否使用标准物质作为质控对照和使用定量标准物质求出相关系数对定量检测结果进行校正。     

大豆中稀土元素分配规律研究

研究了大豆中稀土元素（La、Ce、Nd、Y、Gd）的含量分布规律。结果表明：大豆各部位稀土含量分布一般规律为：根＞茎＞夹壳＞夹果;大豆在生长不同期吸收稀土的能力大小为：幼苗期＞分枝期＞成熟期。总之,稀土元素在大豆中不易迁移,主要集中在根部,果实中含量甚微,因而施用稀土微肥,不会影响食用粮食的安全问题。     

大连转基因检测实验室通过评审

设在大连市产品质量监督检验所内的国家粮食质量监督检验中心,承担粮食及其制品的国家监督抽杏、检验和国家相关标准修订工作。该中心从2002年开始筹建的转基因检测实验室,不久前正式通过了中国实验室国家认可委员会的现场评审。到目前为止,这是我国第一个通过国家实验室认可的转基因检测实验室,能够进行大豆、食用油、玉米、马铃薯等产品的转基因检测工作。     

大豆水溶性蛋白质提取条件优化

通过正交试验方法分析提取温度、提取时间、提取液体积及振荡频率4种因素对大豆水溶性蛋白质测定结果的影响,确定大豆水溶性蛋白质最佳提取条件。结果表明,在一定范围内,大豆水溶性蛋白质含量随着提取温度升高、提取时间延长、提取液体积及振荡频率增大而增大,其中振荡频率对水溶性蛋白质含量的影响达到了显著水平。在已处理样品中加入200 mL提取液,于35℃恒温水浴下以180 r/min回旋振荡120 min时,水溶性蛋白质含量最高。该提取工艺高效、快速、经济,为水溶性蛋白的准确测定以及大豆储存品质的准确判断提供参考。     

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%.     

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.     

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.     

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.     

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.     

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.