邻氨基苯腈气相色谱分析法的研究

采用邻苯二甲酸二壬酯为固定液,Chromsorb W/AW为载体的色谱柱和热导检测器,用苯乙腈为内标物,对邻氨基苯腈试样进行了分析,其中邻氨基苯腈的回收率为100.5%,试样浓度小于1%时测定的相对标准偏差小于8.6%。     

Sweet pregnane glycosides from Telosma procumbens

An intensely sweet polyoxypregnane glycoside, telosmoside A15 (15), was isolated from an Asian Asclepiadaceae plant, Telosma procumbens, collected in Vietnam. This is the first time a sweet pregnane glycoside has been found, and its sweetness intensity is 1000 times greater than that of sucrose. From the same plant, 17 other new glycosides were isolated, having the same aglycone; they are named telosmosides A1-A14 (1-14) and A16-A18 (16-18). Some of these glycosides are also sweet, but others are tasteless or bitter. Chemical structures of the 18 glycosides were determined, and the structure-taste relationship was discussed.     

超高效液相色谱-串联质谱法检测蔬菜中除虫菊素残留

建立了蔬菜中除虫菊素的超高效液相色谱-串联质谱(UPLC-MS/MS)快速检测技术。采用乙腈提取,盐析后无需净化,直接进样分析,正离子多反应监测(MRM)模式测定。结果表明,6种除虫菊素的线性关系良好,相关系数为0.999 5~0.999 9,在0.05、0.1、0.5 mg/kg 3个加标水平下,6种物质的平均回收率为73.9%~109.3%,相对标准偏差(RSDs)为0.4%~7.7%;除虫菊素Ⅰ、除虫菊素Ⅱ的定量下限为0.01mg/kg,瓜叶菊素Ⅰ、瓜叶菊素Ⅱ、茉酮菊素Ⅰ和茉酮菊素Ⅱ的定量下限为0.05 mg/kg,定量下限均指除虫菊素总量。结果表明该方法简便、快速、灵敏度高,适用于蔬菜中除虫菊素的快速检测分析。     

Sensitive and selective fluorescence detection of aqueous uranyl ions using water-soluble CdTe quantum dots

Herein we report a fluorescent method for sensitive and selective detection of uranyl ions using CdTe quantum dots functionalized with mercaptopropionic acid, which the fluorescence of the quantum dots could be quantitatively quenched through electron transfer mechanism. The detection limit of the method was estimated to be 4 nM, less than the maximum allowed content of 130 nM for uranyl in drinking water defined by the U.S. Environmental Protection Agency. Furthermore, the probe was successfully applied in detection of uranyl ions in real samples, demonstrating its potential practical applications for monitoring of uranyl ions in environment.     

Analyte-triggered cyclic autocatalytic oxidation amplification combined with an upconversion nanoparticle probe for fluorometric detection of copper(II)

The authors describe an upconversion nanoparticle-based (UCNP–based) fluorometric method for ultrasensitive and selective detection of Cu²⁺. The UCNPs show a strong emission band at 550 nm under near-infrared excitation at 980 nm. The principle of the strategy is that gold nanoparticles (AuNP) can quench the fluorescence of UCNP. In contrast, the addition of L-cysteine (Cys) can induce the aggregation of AuNP, resulting in a fluorescence recovery of the UCNPs. On addition of Cu²⁺, it oxidizes Cys to cystine and is reduced to Cu⁺. The Cu⁺ thusformed can be oxidized cyclically to Cu²⁺ by dissolved O₂, which catalyzes and recycles the whole reaction. Thus, the aggregation of AuNP is inhibited and the fluorescence recovered by Cys is quenched. Under the optimal condition, the quenching efficiency shows a good linear response to the concentrations of Cu²⁺ in the 0.4–40 nM range. The limit of detection is 0.16 nM, which is 5 orders of magnitude lower than the U.S. Environmental Protection Agency limit for Cu²⁺ in drinking water (20 μM). The method has been further applied to monitor Cu²⁺ levels in real samples. The results of detection are well consistent with those obtained by atomic absorption spectroscopy.

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Graphical abstract Gold nanoparticles (AuNP) as a high efficient fluorescence quenching reagent of upconversion nanoparticles (UCNP) were used in a fluorometric method for detection of Cu²⁺ based on a cyclic catalytic oxidation amplification strategy.

     

Combined electrochemiluminescent and electrochemical immunoassay for interleukin 6 based on the use of TiO<Subscript>2</Subscript> mesocrystal nanoarchitectures

A dual-responsive sandwich-type immunosensor is described for the detection of interleukin 6 (IL-6) by combining electrochemiluminescent (ECL) and electrochemical (EC) detection based on the use of two kinds of TiO₂ mesocrystal nanoarchitectures. A composite was prepared from TiO₂ (anatase) mesocages (AMCs) and a carboxy-terminated ionic liquid (CTIL) and then placed on a glassy carbon electrode (GCE). In the next step, the ECL probe Ru(bpy)₃(II) and antibody against IL-6 (Ab₁) were immobilized on the GCE. Octahedral anatase TiO₂ mesocrystals (OAMs) served as the matrix for immobilizing acid phosphatase (ACP) and secondary antibody (Ab₂) labeled with horseradish peroxidase (HRP) to form a bioconjugate of type Ab₂-HRP/ACP/OAMs. It was self-assembled on the GCE by immunobinding. 1-Naphthol, which is produced in-situ on the surface of the GCE due to the hydrolysis of added 1-naphthyl phosphate by ACP, is oxidized by HRP in the presence of added H₂O₂. This results in an electrochemical signal (typically measured at 0.4 V vs. Ag/AgCl) that increases linearly in the 10 fg·mL^?1 to 90 ng·mL^?1 IL-6 concentration range with a detection limit of 0.32 fg·mL^?1. Secondly, the oxidation product of 1-naphthol quenches the ECL emission of Ru(bpy)₃²⁺. This leads to a decrease in ECL intensity which is linear in the 10 ag·mL^?1 to 90 ng·mL^?1 concentration range, with a detection limit of 3.5 ag·mL^?1. The method exhibits satisfying selectivity and good reproducibility which demonstrates its potential in clinical testing and diagnosis.

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Graphical abstract A dual-responsive sandwich-type immunosensor was fabricated for the detection of interleukin 6 by combining electrochemiluminescence and electrochemical detection based on the use of two kinds of TiO₂ mesocrystal nanoarchitectures.

     

裂解气相色谱-质谱法研究壬酸香草酰胺的热裂解

采用在线热裂解/气相色谱-质谱联用技术(Py/GC-MS)对壬酸香草酰胺(PAVA)的热裂解行为进行了研究,在氦气氛围中考察了不同裂解温度和裂解时间对PAVA裂解的影响,通过GC-MS对裂解产物进行定性和半定量分析。结果表明,随着裂解温度的升高,PAVA裂解率快速提高,裂解产物也进一步增多,当裂解温度达到700℃以上时,可裂解出壬酰胺、2-甲氧基-4-甲基苯酚、1-己烯、壬基腈、壬醛等14种产物。同一温度下随着裂解时间的延长,PAVA的裂解率逐步升高,裂解产物发生了进一步的裂解。根据热裂解产物及主要裂解产物的含量变化,初步推断了PAVA的裂解规律。     

水发食品中甲醛含量快速检测的实验研究

利用品红亚硫酸钠溶液与醛类物质反应后颜色深浅与浓度成正比的原理,使用5种标准浓度的甲醛溶液与希夫试剂反应显色后制作标准比色卡。用待测样品显色后的溶液与制作的标准比色卡进行比对,判断甲醛浓度范围。该方法具有现象明显、灵敏准确、药品易得的优点。因此,可用作中学生课外兴趣实验的实施项目,配制的希夫试剂和制作的标准比色卡也可用于家庭检测水发食品中甲醛含量。     

Microcrystal induced emission enhancement of a small molecule probe and its use for highly efficient detection of 2,4,6-trinitrophenol in water

In this contribution, we reported a very simple and small molecule material, 2,5-dimethoxyterephthalaldehyde(DMA). It exhibited a relatively weak fluorescence in solution, while showed a steadily increased green fluorescence with typical aggregation-induced enhanced emission(AIE) effect for forming a cubic-like microcrystal structure in THF-H2 O mixed solvent.The microcrystals presented significantly higher fluorescence than that of amorphous aggregates. The DMA microcrystals suspension showed a good response to 2,4,6-trinitrophenol(TNP) with a LOD of 1.2×10~(-7) M, which is the best result of TNP detection in aqueous solution. Quantum chemical calculation revealed that DMA is a donor(D)-receptor(A) type molecule with methoxy unit as donor and carbonyl moiety as receptor. Its emission arises from an intramolecular charge transfer(ICT) from methoxy units to carbonyl units. NMR indicated that there is a strong hydrogen bond interaction between DMA and TNP.Hydrogen bond interaction can effectively decrease the intermolecular distance of DMA and TNP, which will increase the efficiency of photoinduced electron transfer(PET) and fluorescence resonance energy transfer(FRET), and hence will be advantageous for its selectivity. The microcrystal induced enhanced emission could be generally used for kinds of target molecules analysis.     

Iron-catalyzed boration of allylic alcohols with H3BO3 as an additive

A method for the synthesis of allylboronates by iron-catalyzed boration of allylic alcohols with H₃BO₃ as an additive is developed. The introduction of H₃BO₃ promotes the cleavage of C?O bond in allylic alcohols obviously. Functional groups, such as fluoro, chloro, bromo, alkyl, and alkoxy, are tolerated well. Thus, various allylboronates are obtained in acceptable yield.