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PHASE HOLDUP AND LIQUID DISPERSION IN GAS-LIQUID-SOLID CIRCULATING FLUIDIZED BEDS
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作者 韩社教 周俭 +1 位作者 金涌 汪展文 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 1997年第3期58-65,共8页
Axial and radial profiles of gas and solids holdups have been studied in agas-liquid-solid circulating fluidized bed at 140mm i.d..Experimental results indicate that the axialand radial profiles of gas and solids hold... Axial and radial profiles of gas and solids holdups have been studied in agas-liquid-solid circulating fluidized bed at 140mm i.d..Experimental results indicate that the axialand radial profiles of gas and solids holdups are more uniform than those in a conventionalfluidized bed.Axial and radial liquid dispersion coefficients in the gas-liquid-solid circulating fluidizedbed are investigated for the first time.It is found that axial and radial liquid dispersioncoefficients increases with increaes in gas velocity and solids holdup.The liquid velocity has littleinfluence on the axial liquid dispersion coefficient,but would adversely affect the redial liquiddispersion coefficient.It can be concluded that the gas-liquid-solid circulating fluidized bed hasadvantages such as better interphase contact and lower liquid dispersion along the axial directionover the expanded bed. 展开更多
关键词 phase HOLDUP liquid dispersION CIRCULATING fluidized BED
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Determination of seven active components in Salvia miltiorrhiza herb by matrix solid phase dispersion combined with ion liquid extraction followed by high performance liquid chromatography
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作者 Bo Hong Yanping Wang +1 位作者 Yinglong Han Wenjing Li 《Asian Journal of Traditional Medicines》 CAS 2021年第2期83-97,共15页
A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet de... A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet detection(UV)is proposed,and it was applied to determine the seven active compounds in Salvia Miltiorrhiza herb.SGSIL and ionic liquid[BMIM]BF4 were used as the adsorbent and the green elution reagent in the MSPD procedure.Several extraction conditions including type of filler and elution solvent,the volume of elution solvent,material liquid ratio were optimized.Under the optimum conditions,the SGSIL-MSPD-HPLC method showed a low limit of detection(LOD,S/N=3)of 0.0122-0.8788μg/mL for standard solution,limit of quantification(LOQ,S/N=10)of 0.0406-2.9292μg/mL for standard solution,wide linear range from 1.56 to 2000μg/mL for all compounds for standard solution,correlation coefficients(r)of more than 0.9990,acceptable reproducibility(relative standard deviations,RSDs<3.54%),and precision of RSDs<3.36%for intra-day,RSDs<3.50%for inter-day.The satisfactory recoveries ranged from 96.4 to 102.5,with RSDs less than 3.45%.The developed SGSIL-MSPD method is easier and more suitable for the determination of the seven active compounds in Salvia Miltiorrhiza herb than the traditional ultrasonic extraction.It was an effective and efficient method for the extraction and quantification of the seven active compounds in traditional Chinese herbal samples. 展开更多
关键词 high performance liquid chromatography(HPLC) silica gel supported ionic liquid(SGSIL) matrix solid phase dispersion(MSPD) Salvia miltiorrhiza(SM) DETERMINATION
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Tb(III) Transport in Dispersion Supported Liquid Membrane System with D2EHPA as Carrier in Kerosene 被引量:2
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作者 PEI Liang YAO Bing-hua +1 位作者 WANG Li-ming MA Zhan-ying 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2011年第1期132-139,共8页
The transport of Tb(III) in dispersion supported liquid membrane(DSLM) with polyvinylidene fluoride membrane(PVDF) as the support and dispersion solution including HCl solution as the stripping solution and di(... The transport of Tb(III) in dispersion supported liquid membrane(DSLM) with polyvinylidene fluoride membrane(PVDF) as the support and dispersion solution including HCl solution as the stripping solution and di(2-ethylhexyl) phosphoric acid(D2EHPA) dissolved in kerosene as the membrane solution, has been studied. The effects of pH value, initial concentration of Tb(III) and different ionic strength in the feed phase, volume ratio of membrane solution to stripping solution, concentration of HCl solution, concentration of carrier, different stripping agents in the dispersion phase on the transport of Tb(III) have also been investigated, respectively. As a result, the optimum transport conditions of Tb(III) were obtained, i.e., the concentration of HCl solution was 4.0 mol/L, the concentration of D2EHPA was 0.16 mol/L, the volume ratio of membrane solution to stripping solution was 30:30 in the dispersion phase and pH value was 4.5 in the feed phase. Ionic strength had no obvious effect on the transport of Tb(III). Under the optimum conditions, the transport percentage of Tb(III) was up to 96.1% in a transport time of 35 min when the initial concentration of Tb(IIl) was 1.0× 10 -4 mol/L. The diffusion coefficient of Tb(III) in the membrane and the thickness of diffusion layer between feed phase and membrane phase were obtained and the values were 1.82×10 -8 m2/s and 5.61 um, respectively. The calculated results were in good agreement with the literature data. 展开更多
关键词 dispersion supported liquid membrane Di(2-ethylhexyl) phosphoric acid Terbium(III) dispersion phase Transport flux Transport percentage
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Electrically tunable holographic polymer templated blue phase liquid crystal grating 被引量:2
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作者 何正红 陈超平 +7 位作者 朱吉亮 袁亚超 李燕 胡伟 李潇 李洪婧 陆建刚 苏翼凯 《Chinese Physics B》 SCIE EI CAS CSCD 2015年第6期328-333,共6页
In this paper, we demonstrate an alternative approach to fabricating an electrically tunable holographic polymer tem- plated blue phase liquid crystal grating. This grating is obtained by preforming a polymer template... In this paper, we demonstrate an alternative approach to fabricating an electrically tunable holographic polymer tem- plated blue phase liquid crystal grating. This grating is obtained by preforming a polymer template comprised of periodic fringes, and then refilling it with a blue phase liquid crystal. Compared with conventional holographic polymer dispersed liquid crystal gratings, our grating can remarkably reduce its switching voltage from 200 V to 43 V while maintaining a sub-millisecond response time. The holographic polymer templated blue phase liquid crystal (HPTBPLC) grating is free from electrode patterning, thus leading to a lower cost and more flexible applications. 展开更多
关键词 holographic polymer dispersed liquid crystal blue phase phase grating
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Prediction of dispersed phase holdup in pulsed disc and doughnut solvent extraction columns under different mass transfer conditions 被引量:3
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作者 Yong Wang Kathryn H.Smith +3 位作者 Kathryn Mumford Teobaldo F.Grabin Zheng Li Geoffrey W.Stevens 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2016年第2期226-231,共6页
Using experimental data from a number of pulsed disc and doughnut solvent extraction columns, a unified correla- tion for the prediction of dispersed phase holdup that considers the effects of mass transfer is present... Using experimental data from a number of pulsed disc and doughnut solvent extraction columns, a unified correla- tion for the prediction of dispersed phase holdup that considers the effects of mass transfer is presented. Pulsed disc and doughnut solvent extraction columns (PDDC) have been used for a range of important applications such as ura- nium extraction and nuclear fuel recycling. Although the dispersed phase holdup in a PDDC has been presented by some researchers, there is still the need to develop a robust correlation that can predict the experimental dispersed phase holdup over a range of operating conditions including the effects of mass transfer direction. In this study, dis- persed phase holdup data from different literature sources for a PDDC were used to refit constants for the correlation presented by Kumar and Hartland lind. Eng. Chem. Res.,27 (1988),131-138] which did not consider the effect of col- umn geometry. In order to incorporate the characteristic length of the PDDC (i.e. the plate spacing), the unified cor- relation for holdup proposed by Kumar and Hartland based on data from eight different types of columns [Ind. Eng. Chem. Res.,34 (1995) 3925-3940] was refitted to the PDDC data. New constants have been presented for each hold- up correlation for a PDDC based on regression analysis using published holdup data from PDDCs that cover a range of onerating conditions and nhwical nronerties and consider the direction of mass transfer. 展开更多
关键词 Solvent extraction liquid extraction Pulsed disc and doughnut columns Solvent extraction column design Holdup dispersed phase holdup Hydrodynamics of extraction columns
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Preparation of Microcapsules with Liquid Droplet Coalescence Method Followed by Phase Separation 被引量:3
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作者 Yasushi Yokoyama Kiyomi Fuchigami +1 位作者 Yoshinari Taguchi Masato Tanaka 《Journal of Encapsulation and Adsorption Sciences》 2013年第3期93-97,共5页
Novel preparation method of microencapsules was developed on the basis of the liquid coalescence method followed by phase separation. Oil droplets of limonene dissolving expanded polystyrene as a shell material were f... Novel preparation method of microencapsules was developed on the basis of the liquid coalescence method followed by phase separation. Oil droplets of limonene dissolving expanded polystyrene as a shell material were forced to collide and coalesce with the Isopar oil droplets of core material in the continuous wates phase. When two kinds of oil droplets are collided and coalesced with each other, expanded polystyrene dissolved in the limonene oil may be phase-separated in the oil droplets newly formed to form the microcapsule shell, because the Isopar oil was a poor solvent for expanded polystyrene but a good solvent for the limonene oil. In the experiment, the diameter (or number) of limonene oil droplets dissolving expanded polystyrene was mainly changed, because the coalescence frequency between the droplets is strongly dependent on the number of droplets. Favorable core shell types of microcapsules with the shell thickness from 1.0 to 5.0 μm were able to be prepared under all the experimental conditions adopted here. 展开更多
关键词 Core Shell MICROCAPSULE liquid DROPLET COALESCENCE METHOD phase Separation LIMONENE Oil liquid-liquid dispersion
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Study on phase retardation characteristic of LCVR using dispersion analysis and SVM 被引量:4
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作者 HU Dongmei LIU Quan +2 位作者 NIU Guocheng ZHU Yifeng YU Lintao 《Instrumentation》 2015年第2期11-17,共7页
To calibrate the phase retardance of a Liquid crystal variable retarder(LCVR),its birefringence dispersion characteristic was analyzed,and the Support vector machines(SVM) algorithm was adopted to establish the predic... To calibrate the phase retardance of a Liquid crystal variable retarder(LCVR),its birefringence dispersion characteristic was analyzed,and the Support vector machines(SVM) algorithm was adopted to establish the prediction model.The obtained SVM decision function was used as a part of LCVR phase retardance,which was generated by the driving voltage.The experimental verification was carried out with a 568 nm laser.The results show that the deviation of the experimental value and the theoretical value is about 0.0061λ.SVM method could be used as an effective method for LCVR phase retardance characteristic calibration. 展开更多
关键词 liquid crystal variable retarder(LCVR) birefringence dispersion support vector machines(SVM) phase retardance calibration
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Matrix Solid-phase Dispersion Extraction of Alkaloids from the Roots of Aconitum kusnezoffii Reichb 被引量:2
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作者 WEI Wei LI Xu-wen SHI Xiao-lei ZHOU Hong-yu YANG Rui-jie ZHANG Han-qi JIN Yong-ri 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2011年第1期23-27,共5页
Matrix solid-phase dispersion(MSPD) was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determina... Matrix solid-phase dispersion(MSPD) was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determination of the analyte was carried out by high performance liquid chromatography with UV detection. The alkaline alumina was used as sorbent. The mixture of acetonitrile and water was used as elution solvent. Several extraction parameters, such as type of sorbent, the ratio of sample to solid support material, type of the elution solvent and the volume of the elution solvent were tested. Mean recoveries ranged from 93.16% to 102.73%, with relative standard deviations from 0.27% to 4.17%. With the extraction efficiency and time expenditure taken into account, MSPD extraction should be a comparatively good method. 展开更多
关键词 Matrix solid-phase dispersion Aconitine-type alkaloid Aconitum kusnezoffii Reichb. EXTRACTION High-performance liquid chromatography 1005-9040(2011 )-01-023-05
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PREPARATION OF POLYMER DISPERSED LIQUID CRYSTALS USING PHOTOPOLYMERIZATION
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作者 Yasuo Hatate 《Chinese Journal of Polymer Science》 SCIE CAS CSCD 2001年第3期311-315,共5页
2-Hydroxyethyl methacrylate (HEMA) and styrene copolymers are prepared by photopolymerization. The electrooptical behavior and microstructure of the polymer dispersed liquid crystal films are investigated by using He-... 2-Hydroxyethyl methacrylate (HEMA) and styrene copolymers are prepared by photopolymerization. The electrooptical behavior and microstructure of the polymer dispersed liquid crystal films are investigated by using He-Ne laser and scanning electron microscopy, respectively. With increasing E7 content in the copolymer, droplet size increased, threshold voltage decreased. 展开更多
关键词 electro-optical properties phase separation polymer dispersed liquid crystal
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分散固相萃取净化-超高效液相色谱-串联质谱法测定蜂蜜中双甲脒、杀虫脒及其代谢物
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作者 王丽 魏茂琼 +4 位作者 康虹钰 陈兴连 兰珊珊 张学艳 刘宏程 《食品与发酵工业》 CAS CSCD 北大核心 2024年第8期284-289,共6页
该研究建立了分散固相萃取-超高效液相色谱-串联质谱(dispersive solid phase extraction-ultra-performance liquid chromatography,UPLC-MS-MS)检测蜂蜜中双甲脒、杀虫脒及其代谢物残留的分析方法。蜂蜜样品2 g加入10 mL水溶液充分混... 该研究建立了分散固相萃取-超高效液相色谱-串联质谱(dispersive solid phase extraction-ultra-performance liquid chromatography,UPLC-MS-MS)检测蜂蜜中双甲脒、杀虫脒及其代谢物残留的分析方法。蜂蜜样品2 g加入10 mL水溶液充分混匀,经1%(体积分数)氨化乙腈超声辅助提取后离心,利用N-丙基乙二胺、C18、氨基键合硅胶混合材料进行分散固相萃取净化,采用ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱分离,以甲醇和0.1%(体积分数)甲酸水溶液为流动相进行梯度洗脱,多反应监测模式正离子扫描分析。6种农药及其代谢物平均回收率为84.1%~113.8%,相对标准偏差为0.9%~6.0%,检出限为0.2~0.8μg/kg,定量限为0.7~2.5μg/kg。实验结果表明该方法快速简便、灵敏度高,适用于蜂蜜中双甲脒、杀虫脒及其代谢物残留同时分析。 展开更多
关键词 蜂蜜 双甲脒 杀虫脒 代谢产物 分散固相萃取 超高效液相色谱-串联质谱
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磁分散固相萃取-高效液相色谱法检测人体尿样中天麻素
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作者 陈晓兵 李慧文 +4 位作者 沙鸥 戴欣成 吴赟帆 徐梓舜 王滋文 《化学研究与应用》 CAS 北大核心 2024年第8期1929-1934,共6页
建立了一种磁分散固相萃取技术结合高效液相色谱法,用于快速检测人体尿液样本中的天麻素。采用化学共沉淀法自组装制备磁性活性炭/大孔树脂三元复合材料(Fe_3O_(4)/AC/MR),并将该材料用作吸附剂,实现尿液样本中天麻素的分离富集。在最... 建立了一种磁分散固相萃取技术结合高效液相色谱法,用于快速检测人体尿液样本中的天麻素。采用化学共沉淀法自组装制备磁性活性炭/大孔树脂三元复合材料(Fe_3O_(4)/AC/MR),并将该材料用作吸附剂,实现尿液样本中天麻素的分离富集。在最佳实验条件下,天麻素浓度与峰面积间呈良好线性关系,线性范围为3.0×10^(-2)~10.0μg·mL^(-1),线性相关系数为0.9994,检出限为5.4μg·L^(-1)。以模拟人体尿液作为实际样品进行加标回收验证,加标回收率为94.87%~106.3%,相对标准偏差(RSD)在2.8%-4.2%之间。本研究建立的方法简便、快速、有效,为生物样本中天麻素的分离提纯提供了新方法。 展开更多
关键词 天麻素 化学共沉淀 磁分散固相萃取 高效液相色谱法 生物样本
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基于分散固相萃取-超高效液相色谱-串联质谱法的大豆农药残留测定研究
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作者 边广 《食品安全导刊》 2024年第16期76-78,共3页
本研究建立了一种分散固相萃取-超高效液相色谱-串联质谱测定吡虫啉、烯啶虫胺等6种常见农药残留的方法。方法学验证结果显示,所有农药的标准曲线线性良好(R^(2)>0.999),方法灵敏度良好;加标回收试验中不同加标浓度的相对标准偏差均... 本研究建立了一种分散固相萃取-超高效液相色谱-串联质谱测定吡虫啉、烯啶虫胺等6种常见农药残留的方法。方法学验证结果显示,所有农药的标准曲线线性良好(R^(2)>0.999),方法灵敏度良好;加标回收试验中不同加标浓度的相对标准偏差均小于10%,验证了方法的稳定性和可靠性。应用此方法对20份市售大豆样品进行农药残留检测,结果显示所有样品中农药残留均未超出或远低于国家规定的最大残留限量,合格率为100%。 展开更多
关键词 分散固相萃取 超高效液相色谱-串联质谱法 大豆 农药残留
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分散固相萃取-液相色谱-串联质谱法测定不同品种柑橘果实不同部位中3种柠檬苦素类似物的含量
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作者 秦芸桦 钟世欢 +5 位作者 陈青俊 王京 王岳 叶佳明 陈云义 孙崇德 《理化检验(化学分册)》 CAS CSCD 北大核心 2024年第2期171-179,共9页
提出了分散固相萃取-液相色谱-串联质谱法同时测定4个品种柑橘果实的4个部位(油胞层、白皮层、囊衣、果肉)中柠檬苦素、诺米林、黄柏酮含量的方法。取5.0 g均质后的样品,加入5 mL水,涡旋混匀后加入20 mL体积比5∶5的丙酮-乙腈混合溶液,... 提出了分散固相萃取-液相色谱-串联质谱法同时测定4个品种柑橘果实的4个部位(油胞层、白皮层、囊衣、果肉)中柠檬苦素、诺米林、黄柏酮含量的方法。取5.0 g均质后的样品,加入5 mL水,涡旋混匀后加入20 mL体积比5∶5的丙酮-乙腈混合溶液,混匀后超声提取10 min,离心5 min。用3 mL水活化2 g EMR-Lipid吸附剂,加至上清液中,涡旋30 s,加入5 g质量比1∶4的氯化钠-硫酸镁混合物和15 mg石墨化碳黑,迅速摇匀后离心1 min。吸取全部上清液,于40℃氮吹至近干,残渣用10.0 mL体积比9∶1的0.1%(体积分数,下同)甲酸溶液和乙腈的混合溶液复溶,过0.22μm滤膜,滤液按照优化的仪器工作条件测定。进行色谱分析时,以CAPCELL PAK ADME HR色谱柱作固定相,以不同体积比的0.1%甲酸溶液和乙腈的混合溶液作流动相进行梯度洗脱分离;进行质谱分析时,以电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式检测。结果显示:3种柠檬苦素类似物的质量浓度在0.10~10.0 mg·L^(-1)内和对应的峰面积呈线性关系,检出限(3S/N)均为0.01 mg·kg^(-1);按标准加入法进行回收试验,回收率为83.1%~90.5%,测定值的相对标准偏差(n=6)为2.6%~5.6%;方法用于30个实际样品的分析,柠檬苦素类似物在不同品种柑橘果实及其不同部位中的含量分布差异显著,柚类品种中柠檬苦素类似物总测定值较高且主要分布在囊衣部位,其他品种主要分布在白皮层和油包层。 展开更多
关键词 分散固相萃取 液相色谱-串联质谱法 柠檬苦素类似物 分布 柑橘果实
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稠油冷采用冻胶分散体调驱体系的相互作用机制
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作者 杨宁 戴彩丽 +3 位作者 邹辰炜 谢忠旭 刘逸飞 赵光 《石油与天然气化工》 CAS CSCD 北大核心 2024年第2期71-77,共7页
目的旨在有效解决稠油化学冷采过程中降黏剂窜流现象严重、油藏动用效率低的问题,支撑稠油绿色高效开发。方法基于稠油冷采降黏剂高效降黏洗油与冻胶分散体调剖剂储层调控的协同效应,采用复配方式构建了稠油冷采用冻胶分散体调驱体系,... 目的旨在有效解决稠油化学冷采过程中降黏剂窜流现象严重、油藏动用效率低的问题,支撑稠油绿色高效开发。方法基于稠油冷采降黏剂高效降黏洗油与冻胶分散体调剖剂储层调控的协同效应,采用复配方式构建了稠油冷采用冻胶分散体调驱体系,测试其基本性能,并使用界面扩张流变仪以及流变仪,考查了体系的界面流变特性和剪切应力特性。结果体系由质量分数为0.06%~0.12%的冻胶分散体和质量分数为0.05%~0.15%的降黏剂组成,为粒径均一的低黏流体,能够降低界面张力并乳化稠油,降黏率达到95%以上。体系中降黏剂在油水界面的吸附行为决定了体系的乳化降黏能力,降黏剂通过吸附在冻胶分散体的表面提高了体系的聚结稳定性,并考查了组分含量及油藏条件对以上过程的影响。结论构建了一种兼具储层调控和高效降黏能力稠油冷采用冻胶分散体调驱体系,探明了体系中各组分间的相互作用机制,为稠油化学冷采提供了技术支持。 展开更多
关键词 稠油冷采 冻胶分散体 乳化降黏 界面流变特性 固-液相互作用
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基于缺陷地慢波传输线结构的液晶移相器设计
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作者 李梓玲 冯燕 +3 位作者 司马博羽 许恒飞 王志诚 吴文 《空军工程大学学报》 CSCD 北大核心 2024年第2期123-127,共5页
为了实现低插损、大相位覆盖范围的加载缺陷地结构(DGS)的微带线液晶移相器,利用HFSS仿真软件对DGS微带线液晶移相器进行建模和仿真,通过改变DGS的形状来改变单个移相单元的色散特性,提升单个单元的移相能力,从而减少移相单元的使用数量... 为了实现低插损、大相位覆盖范围的加载缺陷地结构(DGS)的微带线液晶移相器,利用HFSS仿真软件对DGS微带线液晶移相器进行建模和仿真,通过改变DGS的形状来改变单个移相单元的色散特性,提升单个单元的移相能力,从而减少移相单元的使用数量,降低移相器传输线整体插损。以哑铃型DGS的液晶微带线移相器作为参考标准,比较了5种形状的DGS(哑铃型、减少DGS面积、一阶分形、三角形、交叉型)的移相能力和插损差异。仿真结果表明:下一阶分形和交叉型DGS微带线液晶移相器移相能力较好,最后对不同介电常数的移相器进行仿具观察其S参数和移相能力,进一步验证了这一结果。 展开更多
关键词 缺陷地结构 液晶 移相器 色散 S参数
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亲脂性匹配色谱分离-超高效液相色谱-串联质谱法测定果蔬中21种三唑类杀菌剂 被引量:2
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作者 孟虎 李源槿 +4 位作者 赵丹妮 张雅婷 张丹 杨琦 冯歆轶 《食品工业科技》 CAS 北大核心 2024年第3期293-301,共9页
为了提高农药残留的色谱分离效率和降低基质效应,本研究提出亲脂性匹配色谱分离,选取三唑类杀菌剂为研究对象,建立了果蔬中21种三唑类杀菌剂的超高效液相色谱-串联质谱(Ultra performance liquid chromatography-tandem mass spectromet... 为了提高农药残留的色谱分离效率和降低基质效应,本研究提出亲脂性匹配色谱分离,选取三唑类杀菌剂为研究对象,建立了果蔬中21种三唑类杀菌剂的超高效液相色谱-串联质谱(Ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测方法。样品经乙腈提取,盐析分相,分散固相萃取净化,选用与三唑类杀菌剂具有相近亲脂性的色谱柱进行分离,探究不同亲脂性烷基键合相对基质效应、回收率以及三唑杀菌剂和基质组分色谱分离的影响。结果表明,亲脂性匹配色谱分离能够提高色谱分离效率,改善三唑杀菌剂和基质组分的色谱分离,21种三唑杀菌剂的基质效应为-8.3%~4.7%,在5~250μg/L浓度范围内线性关系良好,决定系数R2≥0.999,平均回收率为91.4%~108.1%,定量限为0.5~3.5μg/kg。该检测方法能够有效降低基质效应,使用溶剂校准曲线进行定量即可获得满意的回收率,显著提高了检测效率,具有简便、准确、灵敏度高等特点,适用于果蔬中三唑杀菌剂的检测。所述亲脂性匹配色谱分离,为农药残留的液相色谱-串联质谱法分析中液相色谱柱的选择和基质效应的降低提供了方法参考。 展开更多
关键词 亲脂性匹配色谱分离 基质效应 三唑类杀菌剂 分散固相萃取 超高效液相色谱-串联质谱
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Fe_(3)O_(4)@AC的制备及其对甲苯磺酸瑞马唑仑分离分析研究
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作者 沙鸥 李慧文 +4 位作者 陈晓兵 戴欣成 吴赟帆 徐梓舜 王滋文 《现代化工》 CAS CSCD 北大核心 2024年第5期247-250,256,共5页
采用超声辅助法制备磁性活性炭复合材料(Fe_(3)O_(4)@AC)并用作磁分散固相萃取剂,同时与高效液相色谱法联用对甲苯磺酸瑞马唑仑进行了分离分析。实验结果表明,在最佳实验条件下,甲苯磺酸瑞马唑仑浓度与峰面积间呈良好线性关系,线性范围... 采用超声辅助法制备磁性活性炭复合材料(Fe_(3)O_(4)@AC)并用作磁分散固相萃取剂,同时与高效液相色谱法联用对甲苯磺酸瑞马唑仑进行了分离分析。实验结果表明,在最佳实验条件下,甲苯磺酸瑞马唑仑浓度与峰面积间呈良好线性关系,线性范围为0.005~1.000μg/mL,线性相关系数为0.999 5,检出限为3.5μg/L。以模拟人体尿液作为实际样品进行加标回收验证,加标回收率为86.1%~106.9%,相对标准偏差(RSD)在2.9%~7.2%之间。 展开更多
关键词 磁分散固相萃取 超声辅助法 甲苯磺酸瑞马唑仑 高效液相色谱法
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分散固相萃取-超高效液相色谱-串联质谱法测定饲料中的多肽类抗生素 被引量:1
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作者 黄燕 李燕妹 +5 位作者 陈言凯 梁敏 冯丽凤 陈何燊 林浩学 蔡小明 《饲料研究》 CAS 北大核心 2024年第5期109-116,共8页
试验基于分散固相萃取净化结合超高效液相色谱-串联质谱法,建立一种同时测定饲料中16种多肽类抗生素(PPTs)的定量分析方法。样品经1%三氯乙酸(aq)-甲醇溶液提取,十八烷基硅胶(C18)分散固相萃取净化后上机测定。在电喷雾正电离模式下,使... 试验基于分散固相萃取净化结合超高效液相色谱-串联质谱法,建立一种同时测定饲料中16种多肽类抗生素(PPTs)的定量分析方法。样品经1%三氯乙酸(aq)-甲醇溶液提取,十八烷基硅胶(C18)分散固相萃取净化后上机测定。在电喷雾正电离模式下,使用多反应监测(MRM)模式,基质匹配校正曲线定量。结果显示,PPTs在相应的浓度范围内线性关系良好,相关系数(R2)大于0.99,检出限为0.4~12.1μg/kg,定量限为1.4~40.4μg/kg。PPTs在饲料中的平均回收率(n=6)为80.0%~114.4%,相对标准偏差(RSD)为2.33%~9.51%。研究表明,该方法操作简单、准确可靠、灵敏度高、分析时间短且重现性高,可广泛应用于饲料中16种PPTs的快速筛查和常规监测。 展开更多
关键词 超高效液相色谱-串联质谱 多肽类抗生素 饲料 分散固相萃取
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基于金属有机骨架多孔碳材料的分散固相萃取-超高效液相色谱-串联质谱法测定水中4种酚类内分泌干扰物
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作者 王盼 马继平 +2 位作者 李爽 程嘉雯 黄超囡 《色谱》 CAS CSCD 北大核心 2024年第3期264-274,共11页
酚类内分泌干扰物是一种干扰内分泌系统的外源性物质,其进入生物体后会干扰细胞的正常功能,引起生殖发育毒性,因此亟需开发一种快速、灵敏的分析方法,用于环境水体中酚类内分泌干扰物的检测。本研究采用溶剂热法合成了一种由金属有机骨... 酚类内分泌干扰物是一种干扰内分泌系统的外源性物质,其进入生物体后会干扰细胞的正常功能,引起生殖发育毒性,因此亟需开发一种快速、灵敏的分析方法,用于环境水体中酚类内分泌干扰物的检测。本研究采用溶剂热法合成了一种由金属有机骨架衍生的多孔碳材料(UiO-66-C),并将其作为萃取吸附剂来富集水中的4种酚类内分泌干扰物(双酚A、4-叔辛基苯酚、4-壬基酚、壬基酚)。建立了一种分散固相萃取(DSPE)结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定水中酚类内分泌干扰物的分析方法。通过扫描电子显微镜、X射线衍射及傅里叶变换红外光谱等测试方法对UiO-66-C进行表征,证明了该材料的成功制备。对DSPE条件进行优化,包括UiO-66-C用量、水样pH、吸附时间、洗脱液种类及体积、洗脱时间和离子强度。在最佳实验条件下,4种酚类内分泌干扰物在0.5~100μg/L范围内线性关系良好,方法检出限和定量限分别为0.01~0.13μg/L和0.03~0.42μg/L,日内和日间精密度分别为1.5%~10.6%和6.1%~13.2%。将该方法应用于自来水和地表水的检测,4种酚类内分泌干扰物的加标回收率为77.1%~116.6%;在自来水样品中未检测到4种酚类内分泌干扰物,而在地表水中检测到微量的4-壬基酚和壬基酚,检出水平分别为1.38μg/L和0.26μg/L。该方法具有良好的准确度和精密度,为环境水体中酚类内分泌干扰物的检测提供了一种快速、高效、灵敏的新途径。 展开更多
关键词 超高效液相色谱-串联质谱 金属有机骨架材料 分散固相萃取 酚类内分泌干扰物 环境水体
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基于改性壳聚糖膜净化的超高效液相色谱-四极杆/静电场轨道阱质谱法测定牛奶中5种兽药残留
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作者 潘旺 张申平 +2 位作者 王安琪 胡军 周丽绘 《色谱》 CAS CSCD 北大核心 2024年第8期758-765,共8页
本研究通过在壳聚糖膜(chitosan membrane,CSM)表面接枝长碳链,获得了十八烷基三甲氧基硅烷改性的壳聚糖膜(C_(18)-CSM),将其作为分散固相萃取吸附剂对牛奶基质进行净化,并结合超高效液相色谱-四极杆/静电场轨道阱质谱(UHPLC-Q/Exactive... 本研究通过在壳聚糖膜(chitosan membrane,CSM)表面接枝长碳链,获得了十八烷基三甲氧基硅烷改性的壳聚糖膜(C_(18)-CSM),将其作为分散固相萃取吸附剂对牛奶基质进行净化,并结合超高效液相色谱-四极杆/静电场轨道阱质谱(UHPLC-Q/Exactive Orbitrap MS)建立了牛奶中氧氟沙星、恩诺沙星、环丙沙星、地西泮和甲硝唑的测定方法。利用扫描电子显微镜、傅里叶变换红外光谱仪和接触角测试仪对C_(18)-CSM材料进行表征。对牛奶样品的前处理条件进行优化,最优条件如下:提取溶剂为5%甲酸乙腈,NaCl用量为1 g,萃取次数为1次,C_(18)-CSM用量为20 mg。采用Hypersil GOLD VANQUISH色谱柱(100 mm×2.1 mm,1.9μm)进行分离,以0.1%甲酸水溶液和0.1%甲酸乙腈作为流动相进行梯度洗脱,流速为0.3 mL/min,进样量为1μL,柱温为25℃,在电喷雾电离源正离子模式下进行检测。在优化的前处理条件下,5种兽药在0.5~100μg/L范围内具有良好的线性关系,相关系数(r^(2))≥0.9970,检出限(LOD)为0.2μg/L,定量限(LOQ)为0.5μg/L。5种兽药在3个加标水平(0.5、1、5μg/L)下的回收率为79.5%~115%,日内精密度为7.0%~13%(n=6),日间精密度为1.3%~11%(n=3)。实验结果表明,本文所建立方法操作简便,准确可靠,能够满足牛奶中5种兽药残留的同时检测。 展开更多
关键词 壳聚糖膜 分散固相萃取 超高效液相色谱-四极杆/静电场轨道阱质谱 兽药残留 牛奶
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