SYNTHESIS OF SALICYLTHIOAMIDES AND 4 H-1, 3, 2 BENZOXAZAPHOSPHORIN-DERIVATIVES

Abstract

Recent studies have shown that the dimer of p-methoxyphenylthionophosphinesulfide, 1, is a very superior thiation reagent, as ketones, amides, and esters are in most cases quantitatively converted to their thio-analogues.     

Br-掺杂Bi2WO6的水热法合成及其可见光催化性能

以Bi（NO₃）₃·5H₂O和Na₂WO₄·2H₂O为主要原料,采用水热法合成了纯相Bi₂WO₆,并对其进行非金属离子Br^-掺杂改性。采用XRD、SEM、TEM、XPS、Raman、PL和DRS研究了Br^-掺杂对Bi₂WO₆的物相结构、形貌和可见光催化性能的影响。结果表明,Br^-掺杂可有效提高Bi₂WO₆的可见光催化性能,当掺杂量（物质的量百分数）为8%时,溴掺杂Bi₂WO₆的光催化性能最好,可见光照射40 min后,可降解96.73%的罗丹明-B,与未掺杂Bi₂WO₆相比,其降解率提高了36.32%。     

一种二维多孔窗口型膦酸锆材料的合成及其对不同金属离子的吸附性能

合成了一种二维窗口型膦酸锆材料β-丙氨酸-N,N-双亚甲基膦酸锆(ZrNCP),采用X射线衍射仪、扫描电镜、透射电镜分析了合成产物的相组成和微观结构;利用N2吸脱附试验装置测定了合成产物对不同金属离子的吸附性能,考察了浓度、温度及pH对其吸附性能的影响.结果表明,合成产物内部存在大量分布均匀的微介孔,材料微观形貌为规整片状.随着金属离子半径的增大,ZrNCP对各种金属离子的平衡吸附量(mmol/g)呈逐渐减小趋势.     

Unexpected Isolation of 4‐Isothiocyanatomethylene‐4H‐pyridine‐1‐carboxylic Acid Ethyl Ester as Potential Template in Organic Synthesis

The synthesis of 4‐isothiocyanatomethyl‐pyridine 4 in 36% yield by Hasegawa and Kotani (Japanese patent 49088878, 1974) has spurred us to investigate this preparation in detail. In addition to this compound, 4‐isothiocyanatomethylene‐4H‐pyridine‐1‐carboxylic acid ethyl ester 3 can be isolated. The synthesis of both compounds 3 and 4 were optimized to 75% and 50% yield respectively. Reaction of compound 3 with methylamine gave thiourea derivatives 5, the same product obtained on reacting 4‐isothiocyanatomethyl‐pyridine 4 with methylamine. We succeed in adjusting the reaction conditions to obtain high yield either from compound 3 or isothiocyanate derivatives 4.     

电感耦合等离子体-发射光谱法测定纯锑中硫的含量

建立了用电感耦合等离子体-发射光谱法(ICP-AES)测定锑锭中硫元素含量的分析方法。样品用王水溶解,加入适量的酒石酸作为稳定剂,稀释定容后直接进行ICP-AES分析。硫元素的测定下限为0.0008%;0.20μg/mL的硫标准溶液平行7次进样的相对标准偏差为3.7%。利用所建立的方法,对两个批次的锑锭进行了分析,加标回收率分别为96.0%和100.6%,并与国标分析方法进行了实验数据比对。     

扫帚状氧化铈制备及其对Pt基阳极催化剂催化性能的影响

采用水热合成法,合成了比表面积为175 m²·g^-1,孔径在2~4nm范围内的扫帚状CeO₂。通过微波辅助乙二醇还原氯铂酸法制备了Pt-CeO₂/RGO催化剂,探究扫帚状CeO₂的添加对Pt基催化剂电催化性能的影响。利用X射线衍射仪（XRD）、扫描电镜（SEM）、N₂吸附-脱附、X射线光电子能谱（XPS）对所制备的CeO₂及催化剂进行表征。利用电化学工作站对催化剂进行电化学性能测试。结果表明,催化剂中CeO₂保持原有扫帚状,Pt纳米粒子均匀分布于石墨烯载体表面;当m_RGO∶m_CeO2=1∶2时,添加了扫帚状CeO₂的Pt-CeO₂/RGO催化剂的电催化性能最优,电化学活性表面积为102.83 m²·g^-1,对乙醇氧化的峰值电流密度为757.17 A·g^-1,1 000 s的稳态电流密度为108.17 A·g^-1,对乙醇催化氧化反应的电荷转移电阻最小,活化能最低。     

Development and validation of an LC–MS/MS method for the quantification of artificial sweeteners in human matrices

Artificial sweeteners are widely used as substitutes for sugar. The sweeteners are generally considered safe, however their whereabouts during pregnancy and lactation and the effect on child development are poorly explored. There is a need for new tools to measure these substances during pregnancy and lactation. Here, we describe the development and validation of a sensitive liquid chromatography–tandem mass spectrometry method for the simultaneous quantification of acesulfame, cyclamate, saccharin and sucralose in human plasma, umbilical cord blood, amniotic fluid and breast milk. The samples were prepared by protein precipitation and separated on a Luna Omega Polar C₁₈ column (2.1 × 50 mm, 1.6 μm). Electrospray ionization in negative mode and multiple reaction monitoring were used to monitor the ion transitions. The validated concentration ranges were from 1 to 500 ng/ml (10–500 ng/ml for sucralose). Interassay precisions were all ≤15% and the accuracies were within ±15%. Stability, linearity, dilution integrity, carryover and recovery were also examined and satisfied the validation criteria. Finally, this analytical method was successfully applied on spiked samples of plasma, umbilical cord blood, amniotic fluid and breast milk, proving its suitability for use in clinical studies on artificial sweeteners, including during pregnancy and lactation.