“Anti-Michael” and Michael Additions in the Reactions of 2-Arylmethyliden-1,3-Indandiones with 2-Aminothiophenol

A novel 2-indano[2,3b]-2-ferrocenyl- and 2-indano[2,3b]-2-(p-methoxy-phenyl)[1,5]benzo-2,5-dihydrothiazepine 5a,b (addition Michael/cyclization) (~30.32%), indano[2,3b]-2-ferrocenyl- and 2-(p-methoxyphenyl)[1,4] benzothiazine 4a,b (addition “anti-Michael”/cyclization) (~45.43%), respectively, were obtained by the condensation of 2-ferrocenyl-and 2-(p-methoxy-phenyl)methyliden-1,3-indandiones 1a,b with o-aminothiophenol 2 in the presence of AcOH and HCl. A new “anti-Michael” addition reaction of 1,4-bis-heteronucleophile 2 into 2-arylmethyliden-1,3-indandiones was reported. As a result of this reaction the product 1a,b was obtained. The structures of the resultant compounds were elucidated by IR, 1H and 13C NMR spectroscopy, mass spectrometry, elemental and X-ray diffraction analysis. The in vitro antitumor activity of the obtained products was researched using the following human cancer cell lines: glioblastoma (CNS U-251), prostatic adenocarcinoma (PC-3), chronic myelogenous leukemia (K562), colorectal adenocarcinoma (HCT-15), mammary adenocarcinoma (MCF-7), and small cell lung cancer (SKLU) and the sulforhodamine B (SRB) method. Among these new compounds some thiazine and thiazepine derivatives showed compelling in vitro antitumor effects on cell lines K-562, HCT-15, SKLU-1 and MCF-7.

Effects of Chinese Herb Additive on Milk Yield and Anti-heat Stress Ability of Holstein Cows

[Objective] To explore the effects of Chinese herb additive on milk yield and anti-heat stress ability of Holstein diary cow. [Method] A total of 36 Holstein cows at same parity and with similar milk yield were randomly divided into three groups, namely, control group, Chinese medi- cine group I and Chinese medicine group I1. The cows in the Chinese medicine group I were fed basal diet containing 4% compound Chinese herb additive; those in the Chinese medicine group II were fed basal diet containing 3% compound Chinese herb additive; and those in the control group were fed common basal diet. All cows in the three groups were analyzed comparatively. [Result] Supplementing some compound Chinese herb ad- ditive into basal diet increased milk yield and anti-heat stress ability of Holstein cows, besides, it also decreased cow diseases like cow mastitis. The Chinese medicine group I generated the highest economic benefit of practical production. [ Conclusion] Supplementing Chinese herb additive in- to basal diet is an effective way to relieve heat stress and increase milk yield.

基于氢谱修饰指数的润滑油添加剂抗磨损性能的预测研究

润滑油添加剂对保障机械运行的稳定性和安全性、延长设备的使用寿命、节约能耗具有重要作用,由于通过实验获得数据费时费力,故用定量结构摩擦性能关系研究方法,来获取抗磨损性能数据成为一种简便而高效的方法.为研究酰肼类及磷酸类润滑油添加剂抗磨损性能与结构的关系,定义并建构了新的氢谱修饰指数^(0)H,并计算36个酰肼类及磷酸类分子的电性距离矢量,筛选了M_(2)、M_(3)、M_(21)和M_(59),将这5个结构描述符作为BP神经网络的输入变量,磨损体积量度V s作为神经网络输出变量,用5-3-1的神经网络结构,构建了神经网络法预测模型,模型相关系数0.944,磨损体积量度V s的预测值与文献实验值的平均相对误差为2.61%,优于文献方法结果.结果表明:酰肼类及磷酸类润滑油添加剂抗磨损性能与氢谱修饰指数有良好的非线性关系,影响抗磨损性能的主要因素是分子中原子特性、基团片段的—CH_(3)、—CH_(2)—、>CH—、—O、—N—和—P—等.该研究对指导合成新型抗磨损性能好的化合物分子有理论意义.

抗缪勒管激素诊断多囊卵巢综合征的年龄特异性阈值探讨及应用

目的 探讨抗缪勒管激素(AMH)诊断多囊卵巢综合征(PCOS)的年龄特异性阈值及其诊断效能。方法 收集该院2 187例14~40岁的月经紊乱的患者样本,并采用免疫荧光方法测定血清AMH水平,符合鹿特丹标准患者为PCOS组,反之为对照组。利用广义加性模型(GAMs)和受试者工作特征(ROC)曲线下面积(AUC)确立AMH的年龄区间和对应的阈值。评估各年龄区间AMH诊断PCOS的效能,并与试剂厂商提供的阈值进行比较。结果 基于GAMs模型,AMH预测PCOS的最佳年龄截断值分别为21、28和35岁。在14~<21岁、21~<28岁、28~<35岁和35~40岁年龄组中,AMH诊断阈值分别为8.28、8.02、6.70、3.96 ng/mL;AUC分别为0.97(95%CI:0.93~0.99)、0.97(95%CI:0.95~0.98)、0.98(95%CI:0.95~0.98)、0.99(95%CI:0.98~0.99);灵敏度分别为0.87、0.87、0.91、1.00;特异度分别为0.94、0.93、0.90、0.93。在各年龄组中,PCOS组的AMH水平均高于对照组,差异具有统计学意义(P<0.001)。结论 应用AMH的年龄特异性阈值,可以更好地评估AMH在区分所有年龄段PCOS患者中的价值。

纳米纤维素在摩擦学领域的应用研究进展

纳米纤维素具有多种独特的优良性质,其摩擦学性能十分优越,是新型绿色纳米润滑材料,已在摩擦学领域展现出巨大的应用潜力与发展前景.本文中以纳米纤维素的摩擦学应用研究为主线,概述了纳米纤维素的有关重要特性,详述了纳米纤维素在聚合物增强填料、水基润滑添加剂、润滑油添加剂、润滑脂添加剂以及润滑电活性调控几方面的研究现状,并相应评述了作用原理与机制,指出了各方面研究仍需解决的重要问题,并展望了未来发展方向.

UPLC-DAD同时测定降血压类保健食品中20种非法添加化学药物

采用超高效液相色谱-二极管阵列检测器(UPLC-DAD)建立同时测定辅助降血压类保健食品中20种非法添加化学药物的方法。采用Luna UPLC C18色谱柱(2.1 mm×100 mm,1.6μm),以质量分数为0.2%的磷酸水溶液-乙腈为流动相进行梯度洗脱。流速为0.21 mL/min,柱温为35℃,DAD扫描,检测波长为220 nm,各剂型样品经甲醇提取,通过保留时间和紫外吸收光谱定性,峰面积外标法定量。结果表明:20种药物成分能完全分离,在4~80μg/mL内线性关系良好,回收率为92.3%~104.1%,相对标准偏差(RSD)为1.3%~2.9%。1批阳性样品检出奈比洛尔、乐卡地平、拉西地平,并通过UPLC-MS/MS得到确证。建立的方法操作简便,精密度、稳定性、重复性好,能够达到快速检测降压类保健食品中非法添加化学成分的目的。

浅析祛痘类化妆品中非法添加盐酸美满霉素等10种组分

基于2018—2021年云南省食品药品监督检验研究院开展的国家化妆品安全监督抽检工作中发现的问题,建立了盐酸美满霉素等10种组分的检测方法对150批次宣称祛痘类化妆品进行筛查,发现风险物质,并进行方法学优化和新方法建立。从对宣称祛痘类化妆品中非法添加抗感染类药物风险探索的必要性、方法开发研究现状、试验方案与设计以及研究结果来阐述。在保持科学性、先进性和规范性的基础上,增加实用性和可操作性,为推动加强化妆品中安全性风险物质和禁用组分的管理检验方法的开发和更新提供研究思路和参考。

硫酸钛-钨酸钠复合添加剂对电解铜箔后处理形貌及抗剥离强度的影响

随着电子信息技术的高速发展,高端且精细的电子产品日益增多,对印制电路板(PCB)用电路板铜箔提出了更高的要求,要求铜箔兼有低粗糙度和高抗剥离强度。针对此问题,采用调控电解铜箔后处理添加剂含量的方法,研究了后处理添加剂对铜箔抗剥离强度的影响。采用预处理过的毛箔,在自制的方形电解槽中通直流电,用配制的不同粗化电解液进行微粗化试验。结果表明:硫酸钛浓度增高,铜箔表面瘤点状颗粒的成核趋势会增大。当浓度为0.7 g/L时,抑制晶粒成核,表面粗糙度先降低后升高。0.3 g/L的硫酸钛可以更好的促进成核,抑制晶粒生长,提高抗剥离强度。加入0.05 g/L钨酸钠和0.3 g/L硫酸钛时,深镀能力最优,其抗剥离性能最高可达到0.7 N/mm。与单纯的钨酸钠体系相比,铜箔的抗剥离强度提高了约30.7%,粗糙度提高了约1.9%。钨酸钠和硫酸钛复合会起到一定的深镀能力,随着钨酸钠的加入,铜箔的抗剥落强度提升,粗糙度呈现下降趋势。

油酸甲酯基琥珀酸、单甲酯、双甲酯的合成及防锈性能

以油酸甲酯与马来酸酐(MA)为原料制备了油酸甲酯基琥珀酸酐(ASA)、油酸甲酯基琥珀酸(MSA)、油酸甲酯基琥珀酸单甲酯(MMS)和油酸甲酯基琥珀酸双甲酯(MDS)作为防锈剂,采用气相色谱-质谱联用、电喷雾电离质谱、傅里叶红外光谱、核磁共振氢谱等手段分析确定了4种防锈剂的结构,并考察4种防锈剂在加氢柴油和150SN润滑油基础油中的防锈蚀性能。结果表明:在加氢柴油中,MSA添加质量分数25μg/g时防锈效果能达到无锈级别,MMS添加质量分数50μg/g时的防锈效果能达到无锈级别;在润滑油中,MSA添加质量分数50μg/g时防锈效果能达到无锈级别,MMS添加质量分数50μg/g时防锈效果能达到无锈级别。并且MSA酸值比工业防锈剂T746低100 mgKOH/g, MMS酸值比工业防锈剂T747低50 mgKOH/g,适用于调制酸值要求低的汽轮机油和液压油。

重载变速冲击工况下MoDDP/CaB复合润滑油添加剂的润滑性能

为解决机械设备在恶劣工况下由润滑失效而导致的设备故障甚至安全生产事故问题,进一步提升机械设备的运行稳定性和安全性,研究纳米硼酸钙(CaB)和二烷基二硫代磷酸钼(MoDDP)单一润滑油添加剂和复合润滑油添加剂的减摩抗磨效果,并探究其润滑作用机制。研究结果表明,重载、变速、冲击工况条件下1.5 wt.%MoDDP/3.0 wt.%CaB复合润滑油添加剂具有良好的减摩抗磨效果,与基础油相比,在不同转速下可最大降低65.1%的摩擦因数和80%的磨痕深度,施加50 N冲击载荷时,可分别降低66.7%的摩擦因数和76.5%的磨痕深度。MoDDP/CaB复合润滑油添加剂在润滑过程中能生成包含C-C、Fe_(2)O_(3)、FeB和MoS_(2)的金属化合物层,添加剂中的CaB和MoDDP能够相互促进彼此反应,增加FeB/MoS_(2)润滑膜的生成量,对比单一的添加剂和基础油,复合添加剂具有更好的自修复性能和协同功效,形成具有高承载力的润滑油膜,提高了复合润滑油的抗磨减摩性能。MoDDP/CaB复合润滑油添加剂的制备可以充分综合利用抗氧化剂与极压耐磨剂的稳定、优异润滑特性,研究结果可为复合添加剂的广泛应用提供数据支持和理论支撑。

高效液相色谱-高分辨率四级杆-飞行时间质谱法测定祛痘类化妆品中20种非法添加抗感染类药物

目的:建立了采用高效液相色谱-高分辨率四级杆-飞行时间质谱(HPLC-Q-TOP-MS)法,检测祛痘类化妆品中20种非法添加抗感染类药物的方法。方法:采用Agilent EC-C18色谱柱(3.0×150 mm,2.7μm);流动相为乙腈-0.1%冰醋酸溶液,梯度洗脱;流速为0.3 mL/min;柱温为35℃;电喷雾电离源,正离子模式,根据MassHunter软件提取的保留时间、母离子、碎片离子精确质量等数据,在PCDL软件中构建了非法添加抗感染类药物的筛查数据库。结果:氯霉素和螺内酯在质量浓度100~5000ng/mL范围内,其余18种抗感染药物在质量浓度50~5000 ng/mL范围内线性关系良好(r>0.99),检出限为0.01~0.20μg/g,定量限为0.05~0.80μg/g,回收率为83.7%~108.8%,相对标准偏差(RSD)为1.2%~8.1%。结论:本法操作简单、准确可靠,适用于祛痘类化妆品中20种抗感染药物的快速筛查,为祛痘类化妆品的安全监管提供了强有力的技术支撑。

液相色谱串联质谱法同时测定消毒产品中抗感染药物

目的:建立HPLC-MS/MS同时检测消毒产品中非法添加33种抗感染药物的方法。方法:样品经过乙腈(含0.5%甲酸)超声提取,采用Shim-pack GIST C18色谱柱(2.1 mm×100 mm,2μm)分离,以5 mmol/L乙酸铵缓冲溶液(p H 4.0)-乙腈(含0.1%甲酸)为流动相,梯度洗脱,流速为0.3 mL/min-1,柱温40℃;采用电喷雾离子源(ESI)正、负离子模式,多反应监测(MRM)模式进行检测。通过比较分子离子峰、二级碎片离子峰、色谱保留时间等确定添加的药物。结果:在10~100 ng/mL的线性范围内,所检测的33种抗感染药物相关系数(r)均大于0.99,线性关系良好,该方法的检出限和定量下限分别为0.08~1.0μg/g、0.1~2.5μg/g。平均加样回收率为80.0%~118.0%,RSD为0.1%~3.8%;精密度、重复性试验的RSD在0.66%~11.85%。结论:经方法学验证,所建立的分析方法可靠、灵敏、简便,降低假阴性、假阳性风险,可用于快速检测消毒产品中非法抗感染的药物。

抗紫外助剂改善沥青老化延度的研究

以中海油生产的SZ36-170#沥青为基质沥青,以调入8种抗紫外助剂后形成的混合沥青为研究对象,先经历RTFOT短期热老化,再进行紫外老化,测试混合沥青的延度等指标变化,在此基础上优选出了两种具有抗紫外功能的助剂。筛选出的03#助剂在添加量为0.3%时,15℃延度增幅为58.6%。

Preparation and Tribological Properties of Lanthanum-doped Muscovite Composite Particles as Lubricant Additives in Lithium Grease

Lanthanum-doped muscovite(MC) composite particles(hereinafter abbreviated as La-MC) were prepared by the mechanical solid-state-chemistry-reaction method, followed by surface modification with oleic acid. The microstructure of materials was characterized by SEM, XRD, EDS and FTIR. Furthermore, the friction-reduction and anti-wear properties of MC and La-MC as lubricant additives in lithium grease were evaluated using a four-ball friction and wear tester. The results showed that La(OH)_3 nanoparticles were coated on the surface of muscovite. Both MC and La-MC can effectively improve the friction-reduction and anti-wear properties of lithium grease and La-MC presents better tribological properties than MC. The excellent tribological properties of La-MC can be attributed to the formation of the adsorbed La-MC film and the chemical reaction film mainly composed of Fe_2O_3 and SiO_2 on the worn surface, as well as the catalysis of lanthanum element during the friction process.

Synthesis of Two Novel Additives and Study of Their Tribological Properties in Rapeseed Oil

二新奇的灰更少添加剂 - benzothiazole 衍生物包含硼和氯， OBC 和 BBC，被综合。在在油菜籽的添加剂上油的不同集体比率(RO ) 的 OBC 和 BBC 的 tribological 表演在一台四球的机器上被检验。油样品润滑的更低的钢球的穿的表面借助于扫描电子显微镜学(SEM ) 被分析。测试结果显示出那 OBC， BBC 在底有好溶解度上油，并且能有效地增加基础油的带负担的能力。包含 1.5 m% BBC 的油样品的最大的非抓住负担是 1117 N，它 2.3 倍于基础油的。OBC 和 BBC 能改进禁止性能和基础油的热稳定性的反穿和腐蚀，谁的起始的分解温度在 350 ° C 上面。然而，在不同集中的 OBC 和 BBC 能增加基础油的磨擦系数。油润滑的钢球的 SEM 形态学取样包含 1.5 m% 添加剂似乎比形成的基础油，和疤的更一致、光滑是很浅的。

The Effect of Cerium Dioxide (CeO_2) in an Anti-corrosion and Self-lubricating Coating

The effect of cerium dioxide(CeO_2)as an additive on the structure and properties of a melting type coating has been studied by means of microhardness measurement,scanning electron microscopy and thermal analysis. The results show that cerium dioxide can modify the microstructure and tribological properties of the coating. Model LIC-23 composite coating which contains CeO_2 performs well as a self-lubricating coating in hydrochloric acid solution.

Study the operating conditions on agglomeration of RDX particles in anti-solvent crystallization by using statistical optimization

The unfavorable growth and agglomeration of micro-particles of RDX explosive was almost observed in manufacture process. For preventing of growth of micro-particles and agglomeration in anti-solvent crystallization process, the effect of additives glucose, sucrose and poly ethylene glycol-2000 and wetting solvent of isopropyl alcohol were studied. Taguchi experimental design was used for optimization of the operating conditions. The type of additive, the amount of additive(%wt.), solvent of wetting and wetting time were selected for optimization of the conditions. By using 4 factor and 3 levels, 27 experiments were conducted(L27). Results showed that in the presence of 2 %wt. of sucrose additive and isopropyl alcohol solvent, the agglomerations of particles were decreased so that a decrease 30-50% in the average of particles size was seen. Addition additives were effective in storage container and for reduce the agglomeration of particles during storage. Also, the agglomeration rate of particles was reduced over time at optimized conditions. Imaging optical microscopy, scanning electron microscopy(SEM), and particle size analyzer(PSA) methods were used for particles size analyzing as a response in statistical optimization and quality control of the final product. The sensitivity to some mechanical and shock stimuli on the RDX in presence of sucrose additive was tested and the obtained results showed the insignificant effect of additive on the safety properties of pure RDX.

Study on Tribology Performance of Different Lubricant Additives under Atmospheric Pressure and High Vacuum Conditions

By using PAO-10 as the base oil, the tribological behavior of 11 additives under high vacuum condition was evaluated. By adopting some surface analytical instruments, such as scanning electron microscopy(SEM), energy dispersive spectroscopy(EDS) and X-ray photoelectron spectroscopy(XPS), the tribological mechanisms of these additives were studied. In air, O_2 can react with metal to form metal oxide that can protect the surfaces of rubbing pair during the tribological tests. According to the theory of the competitive adsorption, the function of some active elements is weakened. In a vacuum environment, the additives contributed more to the lubrication performance. The sulfur-containing additives could react with Fe to produce Fe Sx and "M—C" bonds("M" represents metal). They both had contributions to the lubrication. As for the phosphorus-containing additives, they only generated the phosphates during the tests. When the sulfur and phosphorus-containing additives were applied, the generated phosphates and Fe Sx had the primary contribution to the lubrication performance during the tests.

Application of New Polymeric Additive in Detergent for Automatic Dishwasher

This paper described a new type of multifunctional polymer Noverite^(TM) AD810's calcium ion chelating performance, tinted glass soaking test and its application in containing chlorine or enzyme automatic dishwashing detergent gel and powder. Results showed Noverite^(TM) AD810 has good performance in the final formulation on chelation, anti-filming, and anti-spotting, as well as to prevent the growth of scale crystals.

钢筋混凝土中防腐添加剂的研究进展

在钢筋混凝土结构服役过程中,由环境侵蚀因素导致的耐久性问题是制约结构长效服役的重要原因,其中,氯离子侵蚀导致的钢筋锈蚀是引起钢筋混凝土耐久性劣化的主要因素之一。在混凝土内掺加防腐添加剂,可从促进钢筋表面成膜和改善混凝土自身性能(孔隙结构、水化过程、Friedel’s盐生成)等方面提升阻锈能力,近年来逐渐成为研究热点。本文将防腐添加剂分为传统阻锈剂、绿色植物提取物阻锈剂、纳米材料以及矿物掺合料等四类,从材料开发、作用机制、阻锈影响因素等方面对防腐添加剂的研究进行了综述。最后,探讨了防腐添加剂研究中存在的问题,并对未来的研究提出了建议,以期为防腐添加剂能够更好地防治混凝土中的钢筋锈蚀问题提供参考。