氯球接枝双季盐杀菌材料的制备及性能测试

成功制备了氯球接枝双季盐水不溶性固体杀菌材料。其最优合成条件:反应温度为150℃、反应时间为72 h、反应溶剂分别为邻二氯苯和1-氯代正十四烷。在最优合成条件下该杀菌材料磷的接枝率为2.09mmol/g,长链烷基接枝率为0.31 mmol/g。产品分子结构分别用红外光谱分析和热重分析进行了验证。当产品投加质量浓度为20 g/L,杀菌时间为45 min时,杀菌率可达99.9%,重复使用5次后杀菌率仍可达到98%。

双季铵盐-硫酸酯盐两性Gemini表面活性剂的合成及其表面活性

用N,N-二甲基十二胺、环氧氯丙烷、盐酸(摩尔比为2:1:1)一锅煮的方法得到连接基上带有羟基的双季铵盐Gemini表面活性剂,然后与氯磺酸反应将其羟基硫酸化,再用NaOH中和制得白色粉末状的三头基双季铵盐-硫酸酯钠盐两性Gemini表面活性剂.后两步反应产物的总产率为78%,最终产物的熔点为231～233℃.合成产物的结构用元素分析、红外光谱、质谱和核磁共振等手段进行鉴定.经测定,在15℃时该两性Gemini表面活性剂的表面张力为34.5 mN/m,临界胶团浓度为7.2×10-5mol/L.

直链亚烷基三丁基双季鏻盐的合成与性能

采用双分子亲核加成反应,以三丁基膦、1,6-二溴己烷和1,12-二溴十二烷为原料,在一定条件下分别合成了1,6-亚己基双(三丁基溴化鏻)(HBTP)和1,12-亚十二烷基双(三丁基溴化鏻)(DBTP),并对离子液体产物进行结构表征。采用绝迹稀释法评价杀菌性能,结果表明:在相同的药剂浓度及作用时间下,DBTP的杀菌效果最好,质量浓度为20 mg/L、接触时间为0.5 h时,其对腐生菌、硫酸盐还原菌、铁细菌的杀菌率分别为98.40%、96.44%、99.73%。对比实验表明,DBTP的杀菌能力比四羟甲基硫酸鏻(THPS)强。

咪唑啉基双季-季铵盐型缓蚀杀菌剂的合成与性能研究

以1,3-二溴丙烷、三苯基膦和十六烷基氨乙基咪唑啉为原料,合成了一种新型的咪唑啉基双季-季铵盐型缓蚀杀菌剂,并对产物的结构进行了表征。采用平皿计数法测定产物的杀菌性能,结果表明:在药剂用量为3mg/L时,大肠杆菌杀菌率达95%以上;并且通过旋转挂片腐蚀实验方法,对产物的缓蚀性能进行测定,研究了介质温度、缓蚀剂浓度以及腐蚀接触时间对缓蚀效率的影响。

新型双季吡啶醛肟盐HCM的高效液相色谱法质控

为建立新型双季吡啶醛肟盐HCM含量测定的液相色谱分析新方法。采用Agilent ZORBAX SB-C18色谱柱(5μm,4.6 mm×250 mm);流动相为乙腈,0.5%十二烷基硫酸钠缓冲盐(加入0.2%三乙胺,磷酸溶液调节至pH2.5),梯度(1~4 min43%乙腈,4~6 min 43%~51%乙腈,6~30 min 51%乙腈,30~35 min 51%~43%乙腈,35~40 min,43%乙腈)洗脱;流速为1.0 m L/min;检测波长为290 nm;进样体积为20μL;柱温为室温。上述色谱条件下HCM主峰保留时间22.9 min,对称性良好(<1.05),理论塔板数>7 500;且在0.04~0.14 mg/m L的范围内,进样浓度与峰面积呈良好线性关系(r=0.999 9,n=6);检测限为3 ng,定量限为9 ng;仪器精密度、日内、日间精密度及重复性的RSD均小于2%。所建立的液相色谱方法精密度高,准确度好,可用于新型双季吡啶醛肟盐HCM的含量测定及质量控制。

新型两性双子表面活性剂的合成与表面活性研究

以十二烷基叔胺、环氧氯丙烷和氯乙酸为原料,利用两步法合成了双季铵盐羧甲基钠盐新型两性双子表面活性剂,采用元素分析、红外光谱对其结构进行了表征,考察了反应条件对合成反应收率的影响。第一步合成最佳条件为:n(叔胺):n(盐酸盐):n(环氧氯丙烷)为1.0:1.1:1.0,反应时间18 h;第二步合成最佳条件为:n(双季铵盐):n(氯乙酸)为1.0:1.4,反应时间3 h,反应温度40℃,NaOH质量分数为25%,产物收率达96.5%。产物CMC为0.06 mmol/L,γCMC为18.4 mN/m,优于季铵盐阳离子双子表面活性剂及传统两性表面活性剂。

Synthesis and analgesic activities studies on bispiperazinium (BPZ) salts

Selecting compound 97-9-G4 as lead compound, a series of bispiperazinittm salts 5a-h were designed, synthesized and evaluated for their analgesic activities. The results show that phenylethyl group of 97-9-G4 is a crucial pharmacophore; the intro- duction of electron-withdrawing group on benzene ring is favorable to the activity.

Fragmentation Patterns of Diquaternary Dipiperaziniums Containing Dithiocarboxy lGroups by Electrospray Ionization Tandem Mass Spectrometry

Aim To analyze the fragmentation patterns of diquaternary dipiperaziniumscontaining dithiocarboxyl groups. Methods Positive ion electrospray ionization mass spectrometry inconjunction with tandem mass spectrometry (ESI-MS^n) was used. Results The fragment ion [M^(2+) Cl^-]^+ showed characteristic double peaks with high intensity instead of the parent molecular ionbeing detected. And [M^(2+) - CH_3^+ ]^+ ion had relatively low intensity. Meanwhile, [M^(2+) Cl^- -Cl^- - PhCH_2^+ ]^+ species had the highest intensity as the base peak, which was originated from[M^(2+) Cl^- ]^+, The detailed fragmentation mechanisms are supported with the tandem massspectrometry.

Preparation of spiro-type quaternary ammonium salt via economical and efficient synthetic route as electrolyte for electric double-layer capacitor

A spiro-type quaternary ammonium salt, spiro-(1,1′)-bipyrrolidinium tetrafluoroborate(SBP-BF4) was successfully prepared by an economical and efficient three-step process comprising the cyclization reaction of 1,4-dibromobutane and pyrrolidine, and subsequent ion exchange pathway with KOH followed by neutralization reaction via HBF4 in the system of ethanol solution. 1H NMR, 13 C NMR, FI-IR and XPS analyses showed the structure of SBP-BF4. The as-obtained SBP-BF4 was dissolved in AN and used as the electrolyte for supercapacitor. Electrochemical measurements demonstrate that, compared with commercial electrolyte TEMA-BF4/AN, SBP-BF4/AN exhibits high ionic conductivity, lower resistance and improved cycling performance, which is due to its smaller ion size and stable symmetry structure.

Fragmentation patterns of novel dispirocyclopiperazinium dibromides during electrospray ionization mass spectrometry

The fragmentation patterns of a series of dispirocyclopiperazinium dibromides with strong analgesic activity during positive ion electrospray ionization mass spectrometry were analyzed. The [M-Br]^＋ 2 ions showed the characteristic isotopic peaks and were assigned as the molecular ions. The loss of a 44 Dalton unit from 2 produced ion 3 [M-Br-44]^＋ and the loss of HBr from 2 formed ion 4. Besides, the carbamates 1d-1e produced extra ions [M-2Br-33]^＋. The related fragmentation mechanisms were proposed.

Synthesis of a novel class of cyclophosphamide bis-spiropiperazinium salts

Based on the principle of association, a novel class of cyclophosphamide bis-spiropiperazinium compounds was designed and synthesized. A new method of synthesis, separation and purification for this kind of compounds was also developed.

Synthesis and antibacterial characterization of waterborne polyurethanes with gemini quaternary ammonium salt

To obtain an aqueous polymer system with good antibacterial properties, a series of gemini waterborne polyurethanes （GWPU） were designed and synthesized using isophorone diisocyanate, polyoxytetramethylene glycol, poly（ethylene glycol）, L-lysine and a novel L-lysine-derivatized diamine containing gemini quaternary ammonium salt （EG12） without any other organic agent involved in the whole synthetic process. EG12 was first synthesized and characterized with proton nuclear mag- netic resonance spectra and mass spectra. The antibacterial activities of EG12 and GWPU were evaluated by quanti- fying the minimal inhibitory concentration. The results indicated that the gemini quaternary ammonium chain extender EG12 and GWPU showed excellent antibacterial activity against a broad spectrum of gram-positive and gram-negative bacteria. This work provides a new and facile approach to prepare novel antibacterial materials, which could be applied as coatings in various fields to prevent microbial contamination.