Simultaneous determination of trifloxystrobin and trifloxystrobin acid residue in rice and soil by a modified quick,easy, cheap,effective, rugged,and safe method using ultra high performance liquid chromatography with tandem mass spectrometry

A sensitive analytical method for the simultaneous determination of trifloxystrobin and its metabolite trifloxystrobin acid in rice including straw, bran, brown rice and soil was developed by using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The fungicide trifloxystrobin and its metabolite trifloxystrobin acid were extracted using acetonitrile with 1% formic acid v/v and subsequently cleaned up by primary secondary amine, octadecylsilane or graphitized carbon black prior to ultra high performance liquid chromatography coupled with tandem mass spectrometry. The determination of two target compounds was achieved in less than 3 min using an electrospray ionization source in positive mode. The limits of detection were below 0.22 μg/kg and the limits of quantification did not exceed 0.74 μg/kg in all matrices, which were much lower than the maximum residue levels established by the Codex Alimentarius Commission. The overall average recoveries in four matrix at three levels (0.1, 1.0 and 5.0 mg/kg) ranged from 74.2 to 107.4% with a relative standard deviations of less than 7.8% (n = 5) for both analytes. The method was demonstrated to be convenient and reliable for the routine monitoring of trifloxystrobin and its metabolite. The developed method was validated and applied for the analysis of degradation study samples.     

Label-free colorimetric aptasensor for sensitive detection of ochratoxin A utilizing hybridization chain reaction

The combination of high selectivity of aptamer with the peroxidase-mimicking property of DNAzyme has presented considerable opportunities for designing colorimetric aptasensor for detection of ochratoxin A (OTA). The activities of both aptamer (as biorecognition element) and DNAzyme (as signal amplification element) are blocked via base pairing in the hairpin structure. Hybridization chain reaction (HCR) between two hairpin DNAs was employed to further improve the sensitivity of this method. The presence of OTA triggers the opening of the hairpin structure and the beginning of HCR, which results in the release of many DNAzyme, and generates enhanced colorimetric signals, which is correlated to the amounts of OTA with linear range between 0.01 to 0.32 nM, and the limit of detection is 0.01 nM under optimal conditions. OTA in yellow rice wine and wheat flour samples was also detected using this method. We demonstrate that a new colorimetric method for the detection of OTA has been established, which is simple, easy to conduct, label-free, sensitive, high throughput, and cost-saving.     

Controlled Synthesis of N‐Doped Carbon Nanospheres with Tailored Mesopores through Self‐Assembly of Colloidal Silica

Limited strategies have been established to prepare monodisperse mesoporous carbon nanospheres (MCNs) with tailored pore sizes. In this work, a method is reported to synthesize MCNs by combining polymerization of aniline with co‐assembly of colloidal silica nanoparticles. The controlled self‐assembly behavior of colloidal silica enables the formation of uniform composite nanospheres and convenient modulation over mesopores. After carbonization and removal of sacrificial templates, the resultant MCNs possess tunable mesopores (7–42 nm) and spherical diameters (90–300 nm), as well as high surface area (785–1117 m² g^?1), large pore volume (1.46–2.01 cm³ g^?1) and abundant nitrogen moieties (5.54–8.73 at %). When serving as metal‐free electrocatalysts for the oxygen reduction reaction (ORR), MCNs with an optimum pore size of 22 nm, compared to those with 7 and 42 nm, exhibit the best ORR performance in alkaline medium.     

Compounds with inhibitory activity on peristalsis from the seeds of Holarrhena antidysenterica

Eight compounds were isolated from the seeds of Holarrhena antidysenterica Wall.ex A.DC. On the basis of physico-chemical properties and spectroscopic data, holarrhenanan (1) was identified as a new compound, compounds 2–3 were isolated from H. antidysenterica for the first time, and five known compounds were also obtained. Inhibitory effects of some compounds and extracts to the intestinal peristalsis were evaluated. Results showed that the extracts and compounds 4, 6 exhibited remarkable inhibitory effects with tension inhibition rate of 32.77, 32.77% and amplitude inhibition rate of 59.51, 55.98%, respectively on the vitro rabbit intestinal peristalsis.     

A Novel Self‐assembled Nickel(II)‐Cerium(III) Heterotetranuclear Dimer Constructed from N2O2‐type Bisoxime and Terephthalic Acid: Synthesis,Structure, and Photophysical Properties

By self‐assembly of a Salamo‐type ligand H₂L [H₂L = 1,2‐bis(3‐methoxysalicylideneaminooxy)ethane] with Ni(OAc)₂ · 4H₂O, Ce(NO₃)₃ · 6H₂O, and H₂bdc (H₂bdc = terephthalic acid), a novel Ni^II‐Ce^III heterometallic complex, [{Ni(L)Ce(NO₃)₂(CH₃OH)(DMF)}₂(bdc)], was obtained. Two crystallographically equivalent [Ni(L)Ce(NO₃)₂(CH₃OH)(DMF)] moieties lie in the inversion center, and are linked by one bdc^2– ligand leading to a heterotetranuclear dimer, in which the carboxylato group bridges the Ni^II and Ce^III atoms. Moreover, the photophysical properties of the Ni^II‐Ce^III complex were studied.     

Fine-tuning the molecular energy levels by incorporating thiophene units onto the π-backbone of core-expanded naphthalene diimides

A series of core-expanded naphthalene diimides (NDI-DTYM) and thiophene-based derivatives (1a-c) were designed and synthesized to investigate the relationship between molecular structures and the highest occupied molecular orbital (HOMO) energy levels but has little impact on the lowest unoccupied molecular orbital (LUMO) energy levels. The results demonstrated that increasing the number of thiophene units can gradually elevate the HOMO energy levels but had little impact on the LUMO energy levels. The n-channel organic field-effect transistors (OFETs) based on 1b and 1c have demonstrated that these almost unchanged LUMO energy levels are proper to transport electrons.     

基于MP-AES的在线检测技术在地表水中重金属监测中的应用

通过集成在线富集和在线热消解技术,建立了基于微波等离子体原子发射光谱法(MP-AES)的地表水中重金属的在线检测技术,对珠江干流之一的西江水样中重金属元素(Cd,Cu,Cr,Ni,Pb,Fe,Mn和Zn)进行现场同时在线监测。结果表明,该在线检测技术对这些重金属元素的定量检测能力满足地表水环境质量标准(GB 3838-2002)的限量要求;据环境标准样品中重金属元素分析结果,测定值与配制标准值一致;自来水加标样品的回收率为81.5%~102%。该检测技术对重金属的检出限为1.14~5.34μg/L,检测结果的相对标准偏差(RSD)为0.79%~9.4%,方法可满足地表水中重金属的现场、快速、连续、准确监测需求。     

含噻唑、硫醚结构的1,2,4-三唑类化合物的合成及生物活性

以三氟乙酰乙酸乙酯、磺酰氯、水合肼、异硫氰酸苯酯、碘代芳烃、氯乙酸等为原料,设计、合成了7种新型的含噻唑环、硫醚和三氟甲基的1,2,4-三氮唑类化合物,通过¹H NMR、¹³C NMR、¹⁹F NMR和MS等技术手段对新化合物进行了结构表征。 杀菌活性测试表明,化合物6b、6d和6g在浓度为100 mg/L时对纹枯病菌(Rhizoctoniasolani)的抑制率分别为91%、92%和93%。     

新型含2,4-咪唑啉二酮的4-甲基-3-苯基-2-酰亚胺噻唑啉的合成及生物活性

通过酰氯制备异硫氰酸酯,与5-(4-氨基苄基)-2,4-咪唑啉二酮反应合成了含2,4-咪唑啉二酮的N-苯甲酰基-N'-苯基硫脲,然后在三乙胺存在下再与溴丙酮发生碱催化缩合反应以中等以上收率合成了新型含2,4-咪唑啉二酮的4-甲基-3-苯基-2-酰亚胺噻唑啉,它们的化学结构经1H NMR,IR,HR-ESI-MS和化合物3g和4g的X-ray单晶衍射表征,硫脲与溴丙酮的反应机理通过化合物3g和4g的晶体结构得到进一步确证.初步生物活性测定结果表明:部分目标化合物对供试昆虫及菌种显现出良好的抑制活性,如在200 mg/L浓度下化合物3i和4q对小菜蛾的死亡率分别为86%和100%,在50 mg/L浓度下化合物4n对油菜菌核菌的抑制率为82.6%,而它们对油菜和稗草显示出微弱但并不特征的除草活性.     

有机官能团对硅基MSU-X织构性能的影响

采用有机硅氧烷(RTES)与硅氧烷(TEOS)共水解缩聚合成了有机官能化的MSU-1中孔材料(R=甲基,苯基,乙烯基,脲丙基)。当前驱体中RTES与TO64EOS的摩尔比为0.1:0.9时合成R10-MSU-1分子筛,通过现化分析技术证明BA所选有机官能团均能进入分子筛骨架,而且在相同摩尔数的各数有机硅氧烷存在下,由于其反应速率、空间位阻的不同使其对骨架的缩聚程度、孔道和表面性质有不同的影响。利用SAXS实验技术对所合成R10-MSU-1材料结构表面以及由于有机官能团的存在对无机骨架产生的影响进行了研究。SAXS较强的散射强度分布对Porod定理形成负偏离,表明孔和基体之间有明显的界而层存在,并求得界面层的平均厚度。实验证明有机基团的均匀分布于孔道表面而形成有机界面层。SAXS测试还显示上述分子筛呈质量分形特征,其形成过程可能为非平衡非线性的聚集机制。