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1,3-Bis(2-chloroethyl)-1-nitrosourea enhances the inhibitory effect of Resveratrol on 5-fluorouracil sensitive/resistant colon cancer cells 被引量:4
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作者 Dipon Das Ranjan Preet +2 位作者 Purusottam Mohapatra Shakti Ranjan Satapathy Chanakya Nath Kundu 《World Journal of Gastroenterology》 SCIE CAS 2013年第42期7374-7388,共15页
AIM:To study the mechanism of 5-fluorouracil(5-FU)resistance in colon cancer cells and to develop strategies for overcoming such resistance by combination treatment.METHODS:We established and characterized a 5-FU resi... AIM:To study the mechanism of 5-fluorouracil(5-FU)resistance in colon cancer cells and to develop strategies for overcoming such resistance by combination treatment.METHODS:We established and characterized a 5-FU resistance(5-FU-R)cell line derived from continuous exposure(25μmol/L)to 5-FU for 20 wk in 5-FU sensitive HCT-116 cells.The proliferation and expression of different representative apoptosis and anti-apoptosis markers in 5-FU sensitive and 5-FU resistance cells were measured by the MTT assay and by Western blotting,respectively,after treatment with Resveratrol(Res)and/or 1,3-Bis(2-chloroethyl)-1-nitrosourea(BCNU).Apoptosis and cell cycle arrest was measured by 4',6'-diamidino-2-phenylindole hydrochloride staining and fluorescence-activated cell sorting analysis,respectively.The extent of DNA damage was measured by the Comet assay.We measured the visible changes in the DNA damage/repair cascade by Western blotting.RESULTS:The widely used chemotherapeutic agents BCNU and Res decreased the growth of 5-FU sensitive HCT-116 cells in a dose dependent manner.Combined application of BCNU and Res caused more apoptosis in5-FU sensitive cells in comparison to individual treatment.In addition,the combined application of BCNU and Res caused a significant decrease of major DNA base excision repair components in 5-FU sensitive cells.We established a 5-FU resistance cell line(5-FU-R)from 5-FU-sensitive HCT-116(mismatch repair deficient)cells that was not resistant to other chemotherapeutic agents(e.g.,BCNU,Res)except 5-FU.The 5-FU resistance of 5-FU-R cells was assessed by exposure to increasing concentrations of 5-FU followed by the MTT assay.There was no significant cell death noted in5-FU-R cells in comparison to 5-FU sensitive cells after5-FU treatment.This resistant cell line overexpressed anti-apoptotic[e.g.,AKT,nuclear factorκB,FLICE-like inhibitory protein),DNA repair(e.g.,DNA polymerase beta(POL-β),DNA polymerase eta(POLH),protein Flap endonuclease 1(FEN1),DNA damage-binding protein 2(DDB2)]and 5-FU-resistance proteins(thymidylate synthase)but under expressed pro-apoptotic proteins(e.g.,DAB2,CK1)in comparison to the parental cells.Increased genotoxicity and apoptosis were observed in resistant cells after combined application of BCNU and Res in comparison to untreated or parental cells.BCNU increased the sensitivity to Res of 5-FU resistant cells compared with parental cells.Fifty percent cell death were noted in parental cells when 18μmol/L of Res was associated with fixed concentration(20μmol/L)of BCNU,but a much lower concentration of Res(8μmol/L)was needed to achieve the same effect in 5-FU resistant cells.Interestingly,increased levels of adenomatous polyposis coli and decreased levels POL-β,POLH,FEN1 and DDB2 were noted after the same combined treatment in resistant cells.CONCLUSION:BCNU combined with Res exerts a synergistic effect that may prove useful for the treatment of colon cancer and to overcome drug resistance. 展开更多
关键词 5-FLUOROURACIL 1 3-Bis(2-chloroethyl)-1-nitrosourea RESVERATROL COLON cancer Combination therapy
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Decontamination of 2-Chloroethyl Ethyl Sulfide by Pulsed Corona Plasma 被引量:1
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作者 李战国 胡真 +1 位作者 曹鹏 赵红杰 《Plasma Science and Technology》 SCIE EI CAS CSCD 2014年第11期1054-1058,共5页
Decontamination of 2-chloroethyl ethyl sulfide (2-CEES, CH_3CH_2SCH_2CH_2C1) by pulsed corona plasma was investigated. The results show that 212.6 mg/m^3 of 2-CEES, with the gas flow rate of 2 m^3/h, can be decontam... Decontamination of 2-chloroethyl ethyl sulfide (2-CEES, CH_3CH_2SCH_2CH_2C1) by pulsed corona plasma was investigated. The results show that 212.6 mg/m^3 of 2-CEES, with the gas flow rate of 2 m^3/h, can be decontaminated to 0.09 mg/m^3. According to the variation of the inlet and outlet concentration of 2-CEES vapor with retention time, it is found that the reaction of 2-CEES in a pulsed corona plasma system follows the first order reaction, with the reaction rate constant of 0.463 s^-1. The decontamination mechanism is discussed based on an analysis of the dissociation energy of chemical bonds and decontamination products. The C-S bond adjacent to the C1 atom will be destroyed firstly to form CH3CH2S. and .CH2CH2C1 radicals. CH3CH2S. can be decomposed to .C_2H_5 and .S..S can be oxidized to SO_2, while .C_2H_5 can be finally oxidized to CO_2 and H_2O. The C-Cl bond in the .CH_2CH_2C1 radical can be destroyed to form .CH_2CH_2. and .C1, which can be mineralized to CO_2, H_2O and HCl. The H atom in the .CH_2CH_2C1 radical can also be substituted by -C1 to form CHCl_2-CHCl_2. 展开更多
关键词 pulsed corona plasma DECONTAMINATION 2-chloroethyl ethyl sulfide (2-CEES)
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In vitro release of 1,3-bis(2-chloroethyl)-1-nitrosourea sustained-release microspheres and the distribution in rat brain tissues
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作者 Xia Li1, Liping Guo2, Qin Li3 1Central Pharmacy, General Hospital of Chinese People’s Armed Police Forces, Beijing 100039, China 2Department of Pharmaceutics, Zhengzhou Central Hospital, Zhengzhou 450007, Henan Province, China 3Teda International Cardiovascular Hospital, Tianjin 300457, China 《Neural Regeneration Research》 SCIE CAS CSCD 2006年第9期793-796,共4页
BACKGROUND: The implantation of released chemotherapeutic drugs, which takes biodegradable polymer as vector, into the tumor site can get high concentration and release the drug for a long time, it can directly act on... BACKGROUND: The implantation of released chemotherapeutic drugs, which takes biodegradable polymer as vector, into the tumor site can get high concentration and release the drug for a long time, it can directly act on the tumor cells, and reduce the general toxicity. OBJECTIVE: To explore the in vitro and in vivo course of 1,3-bis(2-chloroethyl)-1-nitrosourea (BCNU) sustained-release from BCNU-loaded polylactide (PLA) microspheres (MS) and location in rat brain tissue. DESIGN: A repetitive measurement. SETTING:Central Pharmacy, General Hospital of Chinese People’s Armed Police Forces. MATERIALS: Thirty male SD rats were used. PLA (Mr5000, batch number: KSL8377) was produced by Wako Pure Chemical Inc.,Ltd. (Japan); BCNU (batch number: 021121) by Tianjin Jinyao Amino Acid Co., Ltd.; BCNU-PLA-MS was prepared by the method of solvent evaporation and pressed into tablets (10 mg/tablet). High-performance liquid chromatography (HPLC) Agilent 1100 (USA); LS9800 liquid-scintillation radiometric apparatus (Beckman). Chromatographic conditions: Elite Hypersil ODS2 C18 chromatographic column (5 μm, 4.6 mm×150 mm); Mobile phase: methanol: water (50:50), flow rate was 1.0 mL per minute, wave length of ultraviolet detection was 237 nm, and the inlet amount of samples was 10 μL. METHODS: The experiments were carried out in the experimental animal center of the General Hospital of Chinese Armed Police from May 2004 to July 2005. ① In vitro BCNU-PLA-MS release test: BCNU-PLA-MS was prepared by the method of solvent evaporation, then placed in 0.1 mol/L phosphate buffered solution (PBS, pH 7.4, 37 ℃), part of MS were taken out at 1, 2, 3, 7, 10 and 15 days respectively, and the rest amount of BCNU in MS was determined by HPLC, then the curve of BCNU-PLA-MS release was drawn. ②In vivo BCNU-PLA-MS release and distribution test: The rats were anesthetized, then BCNU-PLA-MS were implanted to the site 1 mm inferior to the cortex of frontal lobe. Five rats were killed postoperatively at 4 hours, 1, 2, 3, 7 and 15 days, the residual MS was removed from the brain tissue. The rest amount of BCNU was determined with HLPC, and the curve of BCNU-PLA-MS release was drawn as compared with the amount of BCNU in the implanted tablets. Besides, brain tissues (1 g) at the implanted side and the contralateral one were obtained respectively, blood sample (0.5 mL) was also collected, 3H-BCNU was counted radioactively in radioactive liquid flash solution. The distributions of BCNU-PLA-MS in normal rat brain tissue and serum were detected. The analysis of variance was applied to compare the intergroup differences of the measurement data. MAIN OUTCOME MEASURES: ① Characteristics of BCNU-PLA-MS release in phosphate buffered solution (PBS) and rat brain tissue; ② Distributions of BCNU-PLA-MS in normal rat brain tissue and serum. RESULTS: ① Release of BCNU-PLA-MS in PBS and rat brain tissue: The BCNU released from BCNU-PLA-MS could be sustained for over 2 weeks both in PBS and brain tissue. In PBS, the released rate of BCNU was over 15% at 24 hours, nearly 50% at 72 hours and over 90% at 15 days. In brain tissue, the released rate was 8% at 4 hours, 16% at 24 hours, 60% at 72 hours, respectively, and BCNU could be sustained released for over 15 days. ② Distributions of BCNU-PLA-MS in normal rat brain tissue and serum: The concentrations of BCNU in the ipsilateral brain tissue were 6 to 70 times higher than those in the contralateral one. The concentrations of BCNU in the ipsilateral brain tissue were obviously higher than those in serum and contralateral brain tissue (F =103.47, P < 0.01). CONCLUSION: BCNU-PLA-MS can increase the drug concentration in targeted brain tissue, decrease that in the non-targeted brain tissue, reduce general toxic and side effects, and have good releasing function. 展开更多
关键词 BCNU MS PLA nitrosourea sustained-release microspheres and the distribution in rat brain tissues chloroethyl
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Synthesis of Novel Derivatives of 1,5-Dihydro-4,6-dithio-1,3,5,2-triazaphosphorine-2-oxide from N,N-bis(2-chloroethyl)diisocyanato Phosphoramide
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《厦门大学学报(自然科学版)》 CAS CSCD 北大核心 1999年第S1期491-491,共1页
关键词 chloroethyl)diisocyanato Phosphoramide Synthesis of Novel Derivatives of 1 5-Dihydro-4 6-dithio-1 3 5 2-triazaphosphorine-2-oxide from N N-bis
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CPVA微球表面接枝对羟基苯磺酸钠及其对茶碱的吸附研究
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作者 吕振艳 王吉 +1 位作者 马媛 门吉英 《现代化工》 CAS CSCD 北大核心 2024年第3期130-135,共6页
通过分子设计将2-氯乙基异氰酸酯(CIC)键合至聚乙烯醇微球(CPVA)表面制得CPVA-CIC,再将对羟基苯磺酸钠(HSS)固载于CPVA-CIC上制得功能微球CPVA-HSS。通过红外光谱(FI-TR)、扫描电子显微镜(SEM)及Zeta电位仪对功能微球进行表征,并考察主... 通过分子设计将2-氯乙基异氰酸酯(CIC)键合至聚乙烯醇微球(CPVA)表面制得CPVA-CIC,再将对羟基苯磺酸钠(HSS)固载于CPVA-CIC上制得功能微球CPVA-HSS。通过红外光谱(FI-TR)、扫描电子显微镜(SEM)及Zeta电位仪对功能微球进行表征,并考察主要因素对接枝微球固载量的影响,探索功能微球CPVA-HSS对茶碱分子的吸附性能及吸附机理。结果表明,通过CIC改性,阴离子单体HSS成功固载于基质CPVA表面,形成功能微球CPVA-HSS。CPVA-HSS对茶碱吸附5 h达到平衡,凭借其强的静电相互作用,pH5时在水溶液中吸附容量可达60 mg/g,随着温度的降低吸附量升高,而随介质盐度的增大吸附容量降低。功能微球的重复使用性较好。 展开更多
关键词 交联聚乙烯醇微球 对羟基苯磺酸钠 接枝微球 茶碱 2-氯乙基异氰酸酯
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硫化零价铁-微生物复合吸附剂对磷酸三(2-氯乙基)酯的吸附-降解机制
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作者 黄鸿 欧阳浩民 +2 位作者 杨依静 李昌霖 陈烁娜 《化工进展》 EI CAS CSCD 北大核心 2024年第8期4704-4713,共10页
氯代有机磷阻燃剂(chlorinated organophosphate flame retardants,Cl-OPFRs)已在环境中被广泛检出,由于其稳定、易迁移及具有生物毒性,因此已成为不可忽视的新兴有机污染物。本文选择环境中检出率较高的磷酸三(2-氯乙基)酯[tris(2-chlo... 氯代有机磷阻燃剂(chlorinated organophosphate flame retardants,Cl-OPFRs)已在环境中被广泛检出,由于其稳定、易迁移及具有生物毒性,因此已成为不可忽视的新兴有机污染物。本文选择环境中检出率较高的磷酸三(2-氯乙基)酯[tris(2-chloroethyl)phosphate,TCEP]为研究对象,以硫化零价铁(S/ZVI)和TCEP耐受降解菌(缓生新鞘氨醇菌,Novosphingobium tardaugens,N_(1))为研究材料,制备S/ZVI-微生物复合吸附剂(S/ZVI-N_(1)),并对其去除TCEP的性能和降解途径进行探究。结果显示,S/ZVI-N_(1)对TCEP的去除符合准一级动力学方程和Langmuir模型,表明该过程主要为单分子层的物理吸附作用,且根据准二级动力学方程的相关系数可知,在反应过程中同样存在化学吸附过程,S/ZVI-N_(1)作用于TCEP 12h,去除率达58.9%,显著高于仅依靠Novosphingobium tardaugens的去除率(32.9%)和仅依靠S/ZVI的去除率(31.2%)。产物分析表明,S/ZVI-N_(1)作用下TCEP较单独零价铁(zero-valent iron,ZVI)作用下降解更彻底,证明复合吸附剂中S/ZVI和Novosphingobium tardaugens之间存在协同作用,其最佳的反应条件为pH 5~7和30~35℃。微观分析显示,微生物和S/ZVI均参与了TCEP的降解。通过产物分析推导,S/ZVI-N_(1)对TCEP主要有2条降解途径,分别为S/ZVI主导的C—Cl键断裂和Novosphingobium tardaugens主导的O—P键断裂,最终生成磷酸三乙酯(triethyl phosphate,TEP)和磷酸(H_(3)PO_(4))。 展开更多
关键词 氯代有机磷阻燃剂 复合吸附剂 微生物降解 硫化零价铁 降解途径 磷酸三(2-氯乙基)酯
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肝细胞核因子-1b在糜烂性毒剂2-氯乙基乙基硫醚诱导急性肺支气管上皮细胞损伤中的作用及其机制 被引量:1
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作者 孔德钦 刘思佳 +7 位作者 刘建豪 马耀 马丞飞 赵昱舜 周嘉恒 师敏婕 李嘉 刘江正 《癌变.畸变.突变》 CAS 2024年第1期1-8,共8页
目的:探讨肝细胞核因子-1b(HNF-1b)在糜烂性毒剂2-氯乙基乙基硫醚(CEES)诱导人源性肺支气管上皮细胞(BEAS-2B)损伤中的作用及其机制。方法:用不同浓度(0、0.4、0.6、0.8、1.0和1.2 mmol/L)的CEES染毒BEAS-2B细胞24 h,使用CCK-8法检测细... 目的:探讨肝细胞核因子-1b(HNF-1b)在糜烂性毒剂2-氯乙基乙基硫醚(CEES)诱导人源性肺支气管上皮细胞(BEAS-2B)损伤中的作用及其机制。方法:用不同浓度(0、0.4、0.6、0.8、1.0和1.2 mmol/L)的CEES染毒BEAS-2B细胞24 h,使用CCK-8法检测细胞活力,光镜下观察细胞形态,分别采用DCFH-DA和MitoSOX荧光探针检测细胞总活性氧(ROS)和线粒体ROS水平。Western blot检测BEAS-2B细胞中HNF-1b蛋白的表达。再利用慢病毒感染技术构建过表达HNF-1b的BEAS-2B细胞系,用1 mmol/L CESS处理24 h后,分别采用CCK-8法测定细胞活力,Annexin V-FITC/PI双染法检测细胞凋亡率,MitoSOX和DHE荧光探针检测线粒体ROS和细胞总ROS水平,JC-1染色法检测线粒体膜电位。结果:与对照组比较,0.6~1.2 mmol/L CEES染毒后细胞活力均降低(P<0.01);细胞形态发生损伤性改变;0.8~1.2 mmol/L CEES染毒后细胞总ROS和线粒体ROS水平均增加(P<0.01);CEES染毒组细胞HNF-1b蛋白表达水平显著下调(P<0.01)。慢病毒转染后,与对照组正常细胞相比,CEES染毒组HNF-1b过表达细胞的细胞活力显著增加(P<0.01),细胞凋亡率降低(P<0.01),线粒体膜电位的损伤缓解,且线粒体ROS和细胞内总ROS水平显著降低(P<0.01)。结论:糜烂性毒剂CEES能够导致肺支气管上皮细胞中HNF-1b表达降低,过表达HNF-1b能够减轻CEES诱导的细胞损伤和凋亡,抑制线粒体功能障碍,其机制可能与抗氧化有关。上述结果提示HNF-1b可能是糜烂性毒剂导致肺损伤的新靶点,激活HNF-1b可能是糜烂性毒剂毒性靶点治疗的新策略。 展开更多
关键词 糜烂性毒剂 2-氯乙基乙基硫醚 肝细胞核因子-1b BEAS-2B细胞 氧化应激
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Seasonal variations of tris (2-chloroethyl) phosphate and cytotoxicity of organic extracts in water samples from Wuhan, China 被引量:1
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作者 Youjian Zhang Wenjuan Zhang +6 位作者 Jian Hou Xian Wang Wenhong Lu Hongyan Zheng Wei Xiong Junling Liu Jing Yuan 《Journal of Environmental Sciences》 SCIE EI CAS CSCD 2019年第2期299-309,共11页
Tris(2-chloroethyl) phosphate(TCEP) is a typical phosphate flame retardant. Its potential adverse health effects have recently aroused concern. We investigated the seasonal variations of TCEP concentrations in the raw... Tris(2-chloroethyl) phosphate(TCEP) is a typical phosphate flame retardant. Its potential adverse health effects have recently aroused concern. We investigated the seasonal variations of TCEP concentrations in the raw, finished and tap water samples from two drinking water treatment plants(DWTPs) in China, and evaluated the cytotoxicity and apoptosis/necrosis of organic extracts(OEs) in water samples. We enriched TCEP and OEs in water samples by solid-phase extraction method. The TCEP concentrations in water samples were determined by gas chromatography–mass spectrometry. Normal human liver cell line L02 was treated with OEs in the water samples, and then the cytotoxicity and apoptosis/necrosis were measured by 3-(4, 5-dimethyithiazol-2-yl)-2,5-diphenyl-tetrazolium bromide assay and flow cytometry, respectively. The results showed that cytotoxicities of OEs in raw water samples from both DWTPs in summer and winter were stronger than those in spring and autumn, cytotoxicity of OEs in finished and tap water samples from both DWTPs in summer and autumn were stronger than those in spring and winter. In all seasons, the maximal concentrations(100 mL water/mL cell culture) of OEs in the raw water samples from both DWTPs induced late apoptosis/necrosis. The reasons for seasonal variations of TCEP in water samples and potential toxic effects of other pollutants in the water samples need to be further investigated. 展开更多
关键词 TRIS (2-chloroethyl) PHOSPHATE CYTOTOXICITY Organic extract Apoptosis NECROSIS
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Influence of morphology on basicity of CeO2 and its use in 2-chloroethyl ethyl sulfide degradation 被引量:2
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作者 陈文明 冉锐 +3 位作者 翁端 吴晓东 钟近艺 韩世同 《Journal of Rare Earths》 SCIE EI CAS CSCD 2017年第10期970-976,共7页
Three CeO_2 samples with different morphologies, i.e., cubes, rods, and spindles, were synthesized and investigated for 2-chloroethyl ethyl sulfide(2-CEES) degradation. The samples were characterized using scanning ... Three CeO_2 samples with different morphologies, i.e., cubes, rods, and spindles, were synthesized and investigated for 2-chloroethyl ethyl sulfide(2-CEES) degradation. The samples were characterized using scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, the Brunauer-Emmett-Teller method, and temperature-programmed CO_2 desorption. It was found that morphologies of CeO_2 could strongly affect the surface properties and the 2-CEES degradation activities. The surface basicity and the continuous 2-CEES degradation activity of spindle-like CeO_2 were much better than those of the other CeO_2 samples, although all the samples had identical chemical compositions. That was benefited by the largest surface area, abundant microcracks, and surface oxygen vacancies of the spindle-like CeO_2. 展开更多
关键词 CeO2 morphology 2-chloroethyl ethyl sulfate degradation chemical warfare agents rare earths
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锆基金属有机骨架材料/活性碳纤维复合材料的制备及其降解性能
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作者 刘其霞 张天昊 +2 位作者 季涛 葛建龙 单浩如 《纺织学报》 EI CAS CSCD 北大核心 2023年第9期134-143,共10页
为改善活性碳材料在芥子气防护过程中存在的吸附易饱和、处置不当易造成二次污染等问题,制备了一种以活性碳纤维(ACF)为基材的新型降解材料。首先利用抽滤法将纳米锆溶胶沉积到ACF表面,随后采用层层自组装法,以ZrCl 4为金属簇、对苯二... 为改善活性碳材料在芥子气防护过程中存在的吸附易饱和、处置不当易造成二次污染等问题,制备了一种以活性碳纤维(ACF)为基材的新型降解材料。首先利用抽滤法将纳米锆溶胶沉积到ACF表面,随后采用层层自组装法,以ZrCl 4为金属簇、对苯二甲酸为有机配体,在纤维表面原位生长锆基金属有机骨架材料(Zr-MOF),最终制备出一种对芥子气模拟剂2-氯乙基乙基硫醚(CEES)有较高降解性能的Zr-MOF/ACF复合材料,综合采用扫描电子显微镜、X射线衍射、比表面积及孔结构分析等手段进行表征,并测试了其对CEES的降解性能和力学性能。结果表明:锆溶胶的引入有效提高了Zr-MOF在ACF表面的负载量,从而提升了所得材料对CEES的降解性能,并且力学性能也获得显著提高;综合考虑样品的降解性能、拉伸强度与制备效率,将经锆溶胶处理后进行15次循环处理的样品定为最佳工艺样品,经过24 h反应后,对CEES的降解率为83.08%,断裂强度为0.40 MPa,相比于酸化处理的活性碳纤维毡,复合材料的拉伸强度提升了80.99%。 展开更多
关键词 锆基金属有机骨架材料 层层自组装法 2-氯乙基乙基硫醚 活性碳纤维 化学战剂
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UPLC-MS/MS法测定酮咯酸氨丁三醇中的一种基因毒性杂质 被引量:1
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作者 侯继鹏 时晓燕 +3 位作者 张业华 王凯 郝贵周 张贵民 《中南药学》 2023年第9期2424-2427,共4页
目的建立UPLC-MS/MS法测定酮咯酸氨丁三醇中的基因毒性杂质2-[4-苯甲酰基-1-(2-氯乙基)-1H-吡咯-2-基]乙酸乙酯。方法色谱柱采用ACQUITY BEH C18柱(2.1 mm×50 mm,1.7μm),流动相为0.1%甲酸溶液-乙腈(60∶40),等度洗脱。采用电喷雾... 目的建立UPLC-MS/MS法测定酮咯酸氨丁三醇中的基因毒性杂质2-[4-苯甲酰基-1-(2-氯乙基)-1H-吡咯-2-基]乙酸乙酯。方法色谱柱采用ACQUITY BEH C18柱(2.1 mm×50 mm,1.7μm),流动相为0.1%甲酸溶液-乙腈(60∶40),等度洗脱。采用电喷雾电离源(ESI),正离子模式采集,多反应监测(MRM)模式。结果2-[4-苯甲酰基-1-(2-氯乙基)-1H-吡咯-2-基]乙酸乙酯在0.0771~1.5410 ng·mL^(-1)内与峰面积线性关系良好,平均回收率在104.4%~108.2%,RSD均小于5%。定量限与检测限分别为0.0771、0.0231 ng·mL^(-1)。结论建立的方法准确、简便、快速、灵敏度高、专属性强,能有效测定酮咯酸氨丁三醇中2-[4-苯甲酰基-1-(2-氯乙基)-1H-吡咯-2-基]乙酸乙酯的含量,为酮咯酸氨丁三醇的质量控制提供参考。 展开更多
关键词 酮咯酸氨丁三醇 基因毒性杂质 2-[4-苯甲酰基-1-(2-氯乙基)-1H-吡咯-2-基]乙酸乙酯 超高效液相色谱-串联质谱
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2-氯乙基乙基醚的无溶剂合成
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作者 吴小春 何勇 +2 位作者 岳志伟 毛业翔 张洪模 《精细化工》 EI CAS CSCD 北大核心 2023年第5期1143-1148,共6页
对2-氯乙基乙基醚的合成工艺进行了无溶剂合成改进。以三乙胺为催化剂,乙二醇单乙醚与二氯亚砜发生氯代反应合成了2-氯乙基乙基醚,产物经饱和碳酸钠溶液碱洗、饱和氯化钠溶液水洗、无水硫酸钠干燥,得到2-氯乙基乙基醚,采用^(1)HNMR和GC... 对2-氯乙基乙基醚的合成工艺进行了无溶剂合成改进。以三乙胺为催化剂,乙二醇单乙醚与二氯亚砜发生氯代反应合成了2-氯乙基乙基醚,产物经饱和碳酸钠溶液碱洗、饱和氯化钠溶液水洗、无水硫酸钠干燥,得到2-氯乙基乙基醚,采用^(1)HNMR和GC-MS对产物结构进行了表征。采用单因素实验考察了投料物质的量比、反应温度和反应时间对产物GC纯度和收率的影响。优化后2-氯乙基乙基醚的合成工艺为n(乙二醇单乙醚)∶n(二氯亚砜)∶n(三乙胺)=1.0∶1.3∶0.3、反应温度为70℃、反应时间为4h。在该工艺下经公斤级中试放大,产品的收率可达90.2%以上、GC纯度达到99.4%以上、含量达到99.2%以上。 展开更多
关键词 2-氯乙基乙基醚 乙二醇单乙醚 二氯亚砜 三乙胺 无溶剂合成 精细化工中间体
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芥子气模拟剂2-氯乙基乙基硫醚的光催化降解 被引量:9
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作者 韩世同 习海玲 +4 位作者 付贤智 王绪绪 丁正新 林志聪 苏文悦 《物理化学学报》 SCIE CAS CSCD 北大核心 2004年第3期296-301,共6页
利用连续流动微反、原位红外和GC/MS等手段考察了芥子气模拟剂2-氯乙基乙基硫醚(2-CEES)在P25TiO2上的光催化降解反应,证实CO2和H2O是这个反应的最终产物.详细的跟踪分析表明,除了CO2和H2O外,在反应的气相混合物中可检测到C2H4、CH3CHO... 利用连续流动微反、原位红外和GC/MS等手段考察了芥子气模拟剂2-氯乙基乙基硫醚(2-CEES)在P25TiO2上的光催化降解反应,证实CO2和H2O是这个反应的最终产物.详细的跟踪分析表明,除了CO2和H2O外,在反应的气相混合物中可检测到C2H4、CH3CHO、CH4、CO、HCl和H2S;少量小分子的羧酸、醚和砜;微量C2H5SC2H5、C2H5S2C2H5、C2H5SC2H4Cl和CH2ClCH2Cl等中间产物;在反应后的催化剂表面可检测到C2H5S2C2H5、C2H5SC2H4OH、C4H9S2C2H5和C2H5S2C2H4OH、SO2-4等物.根据这些结果提出了2-CEES光催化降解的反应机理,推断2-CEES的光催化降解涉及脱氯、C-S键断裂、有机硫化物光聚合和裂解等复杂过程最终转化为CO2和H2O.认为各种硫物种在表面的积聚引起了催化剂的缓慢失活. 展开更多
关键词 芥子气 模拟剂 2-氯乙基乙基硫醚 光催化降解 化学毒剂 化学武器 洗消方法 催化剂活性 反应机理
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气相色谱法测定纺织品中的三种有机磷阻燃剂 被引量:39
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作者 慕俊泽 李宣 +1 位作者 张斌 江丽媛 《色谱》 CAS CSCD 北大核心 2007年第3期389-391,共3页
建立了超声萃取-毛细管气相色谱-氮磷检测器测定纺织品中3种有机磷阻燃剂的方法。正交试验确定超声萃取的优化条件为萃取溶剂丙酮和正己烷的体积比为2:8,萃取时间为40min,溶剂体积为35mL。实验结果表明,三(2-氯乙基)磷酸酯、三邻... 建立了超声萃取-毛细管气相色谱-氮磷检测器测定纺织品中3种有机磷阻燃剂的方法。正交试验确定超声萃取的优化条件为萃取溶剂丙酮和正己烷的体积比为2:8,萃取时间为40min,溶剂体积为35mL。实验结果表明,三(2-氯乙基)磷酸酯、三邻甲苯基磷酸酯和三(2,3-二溴丙基)磷酸酯等3种化合物的线性范围分别为0.3758~36.38mg/L、0.3841~38.41mg/L和15.78~1010mg/L,检测限依次为0.044,0.053和0.82mg/kg。对于上述3种化合物,方法的精密度分别为6.2%,7.7%和6.5%,方法的回收率介于83.2%和115.4%之间。 展开更多
关键词 气相色谱 三(2-氯乙基)磷酸酯 三邻甲苯基磷酸酯 三(2 3-二溴丙基)磷酸酯 纺织品
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超声萃取/气相色谱-质谱联用法对PVC制品中三(2-氯乙基)磷酸酯的快速测定 被引量:27
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作者 徐善浩 邬蓓蕾 +1 位作者 袁丽凤 夏俊 《分析测试学报》 CAS CSCD 北大核心 2010年第9期978-980,共3页
建立了PVC制品中三(2-氯乙基)磷酸酯(TCEP)的超声萃取/气相色谱-质谱联用快速测定分析方法。考察了萃取溶剂、萃取时间和水浴温度等因素对测定的影响。优化的超声萃取条件为以乙酸乙酯为萃取溶剂,萃取时间为60 min,水浴温度为40℃... 建立了PVC制品中三(2-氯乙基)磷酸酯(TCEP)的超声萃取/气相色谱-质谱联用快速测定分析方法。考察了萃取溶剂、萃取时间和水浴温度等因素对测定的影响。优化的超声萃取条件为以乙酸乙酯为萃取溶剂,萃取时间为60 min,水浴温度为40℃。在优化实验条件下,TCEP的质量浓度在0.1~10 mg/L范围内与峰面积呈良好的线性关系,相关系数为0.999 6,方法的定量下限(S/N=10)为0.1 mg/L,回收率为101%~104%,相对标准偏差为0.76%~3.5%。该方法具有线性范围宽、重复性好、准确度高、速度快等特点,可用于PVC制品中TCEP含量的测定。 展开更多
关键词 三(2-氯乙基)磷酸酯(TCEP) 超声萃取 气相色谱-质谱
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混合模式吸附剂固相萃取-气相色谱-质谱法测定皮革中的磷酸三(2-氯乙基)酯 被引量:5
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作者 张伟亚 朱玉玲 +3 位作者 王成云 李丽霞 张珺清 邢钧 《色谱》 CAS CSCD 北大核心 2014年第10期1157-1162,共6页
磷酸三(2-氯乙基)酯(TCEP)是一种皮革生产中常用的加工助剂,其具有致癌、神经毒性和生殖毒性,被欧洲化学品管理局列入禁用的第二批授权物质清单。由于皮革产品基质复杂,采用常用的固相萃取( SPE)方法提取对TCEP的回收率不高。S... 磷酸三(2-氯乙基)酯(TCEP)是一种皮革生产中常用的加工助剂,其具有致癌、神经毒性和生殖毒性,被欧洲化学品管理局列入禁用的第二批授权物质清单。由于皮革产品基质复杂,采用常用的固相萃取( SPE)方法提取对TCEP的回收率不高。Silica-WCX是一种自制的含有羧基与烷基的新型混合模式吸附剂。研究表明,通过在酸性条件下使其羧基保持质子化状态,能有效增强 Silica-WCX 对极性化合物 TCEP 的萃取性能,使 TCEP 的回收率得到明显提高。本文以 Silica-WCX为 SPE材料,建立了测定皮革中 TCEP的 SPE-GC-MS方法。该方法的线性范围为0.10-100.0μg/L,定量限( S/N=10)为44.46 ng/kg,不同添加水平下 TCEP的平均回收率在91.45%-99.98%之间,相对标准偏差( RSD)在4.33%~5.97%之间。该方法简便快捷,灵敏度高,定量限低于欧盟《化学品的注册、评估、授权和限制》( registration,evaluation,authorization and restriction of chemicals,REACH)法规的限量要求,适用于皮革及其制品中 TCEP的测定。 展开更多
关键词 混合模式吸附剂 固相萃取 气相色谱-质谱法 磷酸三(2-氯乙基)酯 皮革
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氮芥苯甲酸糖酯的合成 被引量:9
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作者 任素梅 江涛 季丽 《化学试剂》 CAS CSCD 北大核心 2004年第3期183-184,共2页
用碳酸钠控制pH ,四丁基溴化胺为相转移催化剂 ,将氮芥苯甲酸与溴代乙酰糖 (溴代乙酰葡萄糖、溴代乙酰半乳糖、溴代乙酰乳糖 )反应 ,合成了 3个氮芥苯甲酸糖酯 ,经IR、1
关键词 氮芥苯甲酸 溴代乙酰基糖 相转移催化
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N,N-二(2-氯乙基)芥酸酰胺的合成及其抗肿瘤作用的研究 被引量:3
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作者 秦箐 高明星 +3 位作者 莫德欢 王闻楚 林华 邝晓聪 《时珍国医国药》 CAS CSCD 北大核心 2010年第9期2162-2164,共3页
目的首次合成未见报道的N,N-二(2-氯乙基)芥酸酰胺,探讨其体内外抗肿瘤活性。方法①以芥酸和双(2-氯乙基)胺盐酸盐为原料、吡啶为催化剂合成N,N-二(2-氯乙基)芥酸酰胺,分离纯化后核磁共振谱确证结构;②用N,N-二(2-氯乙基)芥酸酰胺作用于... 目的首次合成未见报道的N,N-二(2-氯乙基)芥酸酰胺,探讨其体内外抗肿瘤活性。方法①以芥酸和双(2-氯乙基)胺盐酸盐为原料、吡啶为催化剂合成N,N-二(2-氯乙基)芥酸酰胺,分离纯化后核磁共振谱确证结构;②用N,N-二(2-氯乙基)芥酸酰胺作用于Tca8113,用倒置显微镜镜下观察其对Tca8113细胞的生长状况的影响,PI染色经流式细胞术分析其杀伤效应;③S180小鼠动物肿瘤模型观察N,N-二(2-氯乙基)芥酸酰胺对肿瘤的体内抑制作用。结果合成出了N,N-二(2-氯乙基)芥酸酰胺并确证了其结构;N,N-二(2-氯乙基)芥酸酰胺于体外0.15~10.0μg/ml的浓度范围对Tca8113有较强的杀伤效应,杀伤率均超过30%,但与浓度递增无明显的正相关,在100.0μg/ml以上的浓度反而杀伤效果不佳;体内抑制S180的生长,剂量为5mg/kg时,抑制作用最好,生命延长率为38.20%,体重平均增长速率为2.45%。结论采用微型合成法能够快速、方便地合成出N,N-二(2-氯乙基)芥酸酰胺;N,N-二(2-氯乙基)芥酸酰胺在在体内外具有明显的抗肿瘤活性。 展开更多
关键词 芥酸 N N-二(2-氯乙基)芥酸酰胺 TCA8113 S180 抗肿瘤作用
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2-乙基乙烯基醚丙烯酸酯的制备及其阴离子聚合 被引量:3
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作者 侯金顺 邓建平 +3 位作者 韩丙勇 刘亚康 孔令超 杨万泰 《北京化工大学学报(自然科学版)》 CAS CSCD 北大核心 2008年第5期64-68,共5页
在相转移催化剂存在下,以2-氯乙烯醚和丙烯酸钠为原料设计合成了双官能团单体2-乙基乙烯基醚丙烯酸酯,研究了相转移剂的种类以及反应条件对反应的影响。结果表明最佳反应条件为:2-氯乙烯醚/丙烯酸钠物质的量比5∶1;反应温度110℃;反应时... 在相转移催化剂存在下,以2-氯乙烯醚和丙烯酸钠为原料设计合成了双官能团单体2-乙基乙烯基醚丙烯酸酯,研究了相转移剂的种类以及反应条件对反应的影响。结果表明最佳反应条件为:2-氯乙烯醚/丙烯酸钠物质的量比5∶1;反应温度110℃;反应时间4 h;以三乙基苄基氯化铵(TEBA)为相转移剂效果最佳。随后在一定的温度下,以1,1-二苯基己基锂(DPHL)为催化剂,以2-乙基乙烯基醚丙烯酸酯为单体在四氢呋喃中进行了阴离子聚合,得到分子量可控的单分散的聚合物。 展开更多
关键词 相转移催化剂 丙烯酸酯衍生物 2-氯乙烯醚 阴离子聚合
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TCEP和环基苯对F型锂离子电池的复合作用 被引量:2
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作者 陈玉红 汪亮 +2 位作者 孙娜 许新芳 唐致远 《电源技术》 CAS CSCD 北大核心 2014年第7期1243-1245,1301,共4页
将磷酸三(β-氯乙基)酯(TCEP)和环基苯(CriB)作为F型(5Ah)锂离子动力电池添加剂以提高电池的耐高温性能同时对电池进行过充保护。循环伏安和环境电子扫描电镜(ESEM)研究结果表明;TCEP分解电压约为4.75V。CHB的氧化聚合电位... 将磷酸三(β-氯乙基)酯(TCEP)和环基苯(CriB)作为F型(5Ah)锂离子动力电池添加剂以提高电池的耐高温性能同时对电池进行过充保护。循环伏安和环境电子扫描电镜(ESEM)研究结果表明;TCEP分解电压约为4.75V。CHB的氧化聚合电位在4.6V左右,被过充电池的LiMnO4正极表面覆盖一层CHB的聚合产物保证了电池过充时的安全性;电解液差热分析(DTA)曲线在260~360℃出现了TCEP的三个分解吸热峰。保证了电池在过热时的安全性;在150℃环境温度下对含5%TCEP和同时含5%CHB和TCEP的电池的耐高温测试中电池均不失控。且后者的耐高温效果优于前者;在1~10V过充实验中发现同时含5%CHB和TCEP电池的过充效果优于单独含有5%CHB的电池;而且TCEP和CHB对电池循环性能和荷电保持能力的影响极小。 展开更多
关键词 锂离子电池 磷酸三(β-氯乙基)酯 环基苯 安全性
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