一类新偶氮试剂的研究：Ⅴ.HQSAH催化荧光法测定Mn（Ⅱ）

基于Ｍｎ（Ⅱ）对试剂２－（８＇－羟基喹啉－５＇－磺基－７＇－偶氮基）－１－羟基－８－氨基一萘二磺酸（以下简称ＨＱＳＡＨ）分解反应的催化作用，提出了锰的荧光催化动力学分析新方法，其λｅｘ／ｅｍ＝２３０／４１５ｎｍ，适宜酸度范围为ｐＨ１１．０～１２．０，Ｍｎ（Ⅱ）含量在０～０．０８μｇ／ｍＬ呈线性关系，该法用于分析铸造铝合金中的痕量锰，效果良好。还初步探讨了反应机制，确定了反应动力学方程，测定了反应速率和活化能。     

Synthesis of a Systematic 64-Membered Heparan Sulfate Tetrasaccharide Library

Heparan sulfate (HS) has multifaceted biological activities. To date, no libraries of HS oligosaccharides bearing systematically varied sulfation structures are available owing to the challenges in synthesizing a large number of HS oligosaccharides. To overcome the obstacles and expedite the synthesis, a divergent approach was designed, where 64 HS tetrasaccharides covering all possible structures of 2-O-, 6-O- and N-sulfation with the glucosamine-glucuronic acid-glucosamine-iduronic acid backbone were successfully produced from a single strategically protected tetrasaccharide intermediate. This extensive library helped identify the structural requirements for HS sequences to have strong fibroblast growth factor-2 binding but a weak affinity for platelet factor-4. Such a strategy to separate out these two interactions could lead to new HS-based potential therapeutics without the dangerous adverse effect of heparin-induced thrombocytopenia.     

高效液相色谱法测定水产品中四环素类抗生素残留

建立了一种高效液相色谱法测定水产品中土霉素、四环素、去甲基金霉素、金霉素、脱氧土霉素的分析方法。样品用5.0%高氯酸溶液提取,上清液用OasisHLB固相萃取柱净化,用紫外检测器于355nm测定。土霉素、四环素、去甲基金霉素检测限为0.01mg/kg,金霉素、脱氧土霉素检出限为0.02mg/kg。5种药物的回收率在74.8%~89.3%之间,相对标准偏差为3.95%~9.95%。方法适用于水产品中四环素类抗生素残留的检测。     

Sensitive Stripping Determination of Cadmium(II) and Lead(II) on Disposable Graphene Modified Screen‐Printed Electrode

In the present work, a sensitive, facile and disposable sensing platform for trace analysis of heavy metal ions was developed at the Bi modified graphene‐poly(sodium 4‐styrenesulfonate) composite film screen printed electrode (GR/PSS/Bi/SPE). The GR/PSS/Bi/SPE improved sensitivity and linearity due to the functionalization of graphene with negatively charged PSS providing more absorbing sites. The detection limit of the GR/PSS/Bi/SPE is found to be 0.042 µg L^?1 for Cd²⁺ and 0.089 µg L^?1 for Pb²⁺ with linear responses of Cd²⁺ and Pb²⁺ in the range of 0.5–120 µg L^?1. Finally, the practical application was confirmed in real water with satisfactory results.     

关于Alzer不等式的一个简单证明

利用数学归纳法和函数的单调性，本给出了Alzer不等式的一个简单证明．     

Separation and quantitative determination of sesquiterpene lactones in Lindera aggregata (Wu‐yao) by ultra‐performance LC‐MS/MS

An ultra‐performance LC in combination with MS/MS method was established to evaluate the quality of Wu‐yao (the dried root of Lindera aggregata (Sims) Kosterm. (Lauraceae)) through simultaneous quantitation of five sesquiterpene lactones, linderagalactone D ( 1 ), linderagalactone C ( 2 ), hydroylindestenolide ( 3 ), neolinderalactone ( 4 ) and linderane ( 5 ). All compounds were separated on a Waters Acquity ultra‐performance LC HSS T3 column (2.1 mm×100 mm, 1.8 μm particle size) with linear gradient elution of acetonitrile and 0.1% formic acid. An ESI interface in the positive mode was employed prior to MS detection. All the compounds showed good linearity (R²≥0.9992). The recoveries, measured at three concentration levels, varied from 97.3 to 103.4% with RSDs <4.8%. The simple, rapid and reliable method was successfully applied to quantify the five components in 13 samples of Wu‐yao from different areas.     

Influence of precipitant solution pH on the structural, morphological and upconversion luminescent properties of Lu2O3:2%Yb, 0.2%Tm nanopowders

Lutetium oxide nanopowders codoped with Tm³⁺ and Yb³⁺ were synthesized by the reverse-strike co-precipitation method. Effects of precipitant solution pH on the structural, morphological and upconversion luminescent properties of Lu₂O₃:2%Yb, 0.2%Tm nanopowders had been investigated. The results show that pH value of the precipitant (NH₄HCO₃) solution has a significant effect on the particle size, morphology and upconversion emission intensity of the Lu₂O₃:2%Yb, 0.2%Tm nanopowders. All the samples obtained from different pH value of precipitant solution can be readily indexed to pure cubic phase of Lu₂O₃, indicating good crystallinity. The upconversion emission intensity of Lu₂O₃:2%Yb, 0.2%Tm nanopowders obtained from the precipitant solution with pH=11 is the strongest. The enhancement of the upconversion luminescence is suggested to be the consequence of reducing the number of OH⁻ groups and the enlarged nanopowder size. The strong blue, weak red and near infrared emissions from the prepared nanopowders were observed under 980 nm laser excitation, and attributed to the ¹G₄→³H₆, ¹G₄→³F₄ and ³H₄→³H₆ transitions of Tm³⁺ ion, respectively.     

Study of total ionizing dose radiation effects on enclosed gate transistors in a commercial CMOS technology

This paper studies the total ionizing dose radiation effects on MOS (metal-oxide-semiconductor) transistors with normal and enclosed gate layout in a standard commercial CMOS (compensate MOS) bulk process. The leakage current, threshold voltage shift, and transconductance of the devices were monitored before and after $\gamma $-ray irradiation. The parameters of the devices with different layout under different bias condition during irradiation at different total dose are investigated. The results show that the enclosed layout not only effectively eliminates the leakage but also improves the performance of threshold voltage and transconductance for NMOS (n-type channel MOS) transistors. The experimental results also indicate that analogue bias during irradiation is the worst case for enclosed gate NMOS. There is no evident different behaviour observed between normal PMOS (p-type channel MOS) transistors and enclosed gate PMOS transistors.     

Simultaneous determination of four alkaloids in Lindera aggregata by ultra-high-pressure liquid chromatography-tandem mass spectrometry

A new separation and quantification method using liquid chromatography under ultra-high-pressure in combination with tandem mass spectrometry (MS/MS) was developed for simultaneous determination of four alkaloids in Lindera aggregata. The analysis was performed on an Acquity UPLC BEH C(18) column (50mmx2.1mm, 1.7microm particle size; Waters, Milford, MA, USA) utilizing a gradient elution profile and a mobile phase consisting of (A) water containing 10mM ammonium acetate adjusted to pH 3 with acetic acid and (B) acetonitrile. An electrospray ionization (ESI)-tandem interface in the positive mode was employed prior to mass spectrometric detection. The calibration curve was linear over the range of 17.1-856ng for boldine, 42.4-2652ng for norboldine, 6.1-304ng for reticuline and 0.5-50ng for linderegatine, respectively. The average recoveries ranged from 99.2 to 101.4% with RSDs< or =2.7%. Then, four L. aggregata samples from different batches were analyzed using the established method. The results indicated that ultra-high-pressure liquid chromatography-tandem mass spectrometry provided improved chromatographic parameters resulting in significantly increased sample throughput including lower solvent consumption and lower limits of quantitation (LOQs) for most of target analytes compared to previous method employing conventional high-performance liquid chromatography (HPLC) separation. So, the established method was validated, sensitive and reliable for the determination of four alkaloids in L. aggregata.     

K9光学玻璃化学钢化技术研究

为提高K9光学玻璃在一些特殊应用领域(如高压、温度变化剧烈等)的力学性能,并保证其光学性能符合精密光学仪器要求,对K9光学玻璃进行了化学钢化技术研究.以脆性材料断裂过程微裂纹扩展理论为基础,导出化学钢化玻璃强度应力因子计算模型,分析化学钢化表面应力与表面微裂纹深度、韧性之间的关系,指出化学钢化工艺应注意的事项.通过实验...