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重液法分离密度差值很小的单矿物的技术及其应用 被引量:2
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作者 张美怡 卢静 《地质通报》 CAS CSCD 北大核心 2010年第11期1726-1729,共4页
介绍了密度差值很小的单矿物的分离技术方法,并利用重液折光率千分位和万分位的细微区别分离单矿物石英和绢云母。该方法由石英与长英质混合物的分离技术,推广到绢云母与绢云母长英质混合物的分离技术,改进后的重液分离技术具有快速、... 介绍了密度差值很小的单矿物的分离技术方法,并利用重液折光率千分位和万分位的细微区别分离单矿物石英和绢云母。该方法由石英与长英质混合物的分离技术,推广到绢云母与绢云母长英质混合物的分离技术,改进后的重液分离技术具有快速、高效、经济的特点。当重液的折光率为1.577~1.580时,石英的分离纯度能达到95﹪~99﹪;当重液的折光率为1.5895~1.5840时,绢云母的分离纯度能达到90﹪~99﹪。 展开更多
关键词 折光率 重液法 密度差值很小的单矿物 单矿物 石英 绢云母 长英质矿物混合体 绢云母长英质混合物
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三重四级杆液质法检测食品中毒黄素和米酵菌酸含量 被引量:1
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作者 赵智锋 王晓琴 +5 位作者 叶文芳 车宇慧 黄秀丽 陈榕德 甘维明 陈嘉聪 《中国农学通报》 2024年第3期128-134,共7页
旨在建立利用三重四级杆液相色谱质谱(UPLC-MS/MS)同时测定食品中毒黄素和米酵菌酸含量的方法。样品在80%甲醇水溶液体系中萃取,离心后上清液经QuEChERS EMR-Lipid净化处理,浓缩、复溶后,以0.1%甲酸水和乙腈为流动相经梯度洗脱,液质电... 旨在建立利用三重四级杆液相色谱质谱(UPLC-MS/MS)同时测定食品中毒黄素和米酵菌酸含量的方法。样品在80%甲醇水溶液体系中萃取,离心后上清液经QuEChERS EMR-Lipid净化处理,浓缩、复溶后,以0.1%甲酸水和乙腈为流动相经梯度洗脱,液质电喷雾离子源正负模式检测,使用外标法进行定量分析。实验结果显示,毒黄素和米酵菌酸在浓度为0.5~100μg/L的范围内表现出较好线性关系,线性线性相关系数r大于0.995,在不同基质多水平添加浓度下,回收率为86.8%~103.6%,相对标准偏差(RSD)小于5%,毒黄素方法检出限为0.1μg/kg,定量限为0.2μg/kg,米酵菌酸方法检出限为0.05μg/kg,定量限为0.1μg/kg。该方法灵敏度高、专属性好、准确可靠,适合食品中毒黄素和米酵菌酸含量的测定。 展开更多
关键词 毒黄素 米酵菌酸 四级杆 QUECHERS
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亲水作用色谱-三重四极杆质谱法分析肉中代谢调节剂美度铵残留 被引量:1
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作者 郑锌 王雨晴 +3 位作者 李莹 李长坤 李月琪 黄涛宏 《环境化学》 CAS CSCD 北大核心 2022年第4期1457-1460,共4页
本文采用亲水作用(HILIC)色谱-串联质谱,建立了肉类中代谢调节剂美度铵残留量的测定方法.肉类样品经碳酸氢铵-乙腈缓冲液提取,HLB固相萃取柱净化,经HILIC色谱分离,三重四极杆质谱多反应监测模式(MRM)测定,基质匹配外标曲线定量.结果显... 本文采用亲水作用(HILIC)色谱-串联质谱,建立了肉类中代谢调节剂美度铵残留量的测定方法.肉类样品经碳酸氢铵-乙腈缓冲液提取,HLB固相萃取柱净化,经HILIC色谱分离,三重四极杆质谱多反应监测模式(MRM)测定,基质匹配外标曲线定量.结果显示,5—1000μg·kg^(-1)浓度范围内线性良好,判定系数r^(2)均大于0.995,线性良好;猪肉、虾中美度铵的检出限分别为0.2、0.3μg·kg^(-1),定量限分别为0.7、1.0μg·kg^(-1),空白样品中加标5、10、50μg·kg^(-1),加标回收率81.8%—109.5%之间.该方法简便,灵敏度高,准确度好. 展开更多
关键词 四极杆质联用 美度铵 肉类 代谢调节剂 兴奋剂
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黄土样品重量对孢粉分析结果的影响 被引量:1
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作者 冯雪冰 魏明建 《首都师范大学学报(自然科学版)》 2015年第5期60-64,67,共6页
黄土地层中,下层由于年代更老,经历更长时间的腐蚀,因此要比上层孢粉损失量更大,如何在下层黄土中提取到足够量的花粉并且保证孢粉分析结果的稳定性成为研究的重点.本文通过对黄土高原第四层黄土和第四层古土壤使用重液浮选法进行前处理... 黄土地层中,下层由于年代更老,经历更长时间的腐蚀,因此要比上层孢粉损失量更大,如何在下层黄土中提取到足够量的花粉并且保证孢粉分析结果的稳定性成为研究的重点.本文通过对黄土高原第四层黄土和第四层古土壤使用重液浮选法进行前处理,以样品重量为变量进行对比实验,应用相关性、多样性和相似性分析方法对孢粉分析结果进行研究,尝试找到最适实验样品重量.结果显示,当样品重量为200 g和250 g时,孢粉质量浓度趋于平稳,误差较小,这一重量区间的结果可信度更高.而物种多样性随样品重量变化的关系不明显,有待进一步实验研究.从鉴定结果的植被组成以及所占百分比含量这方面来看,当样品重量为150 g和200 g时,实验结果更加稳定.总的来说,样品重量在150 g^200 g这一区间时,各项孢粉分析结果更稳定、误差更小. 展开更多
关键词 浮选 黄土 孢粉分析
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南海细粒沉积物孢粉处理方法的对比研究
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作者 刘梓锐 王汝英 陈芳(审稿) 《海洋地质》 2018年第2期74-78,共5页
海洋细粒沉积物中含有丰富的孢粉化石,不同的处理方法对孢粉富集程度的影响亦不同。为寻找简便而又环保的孢粉处理方法,满足我局地勘和科研项目大批量孢粉研究需要,开展氢氟酸重液浮选法和酸碱过筛法两种不同方法在富集孢粉方面的优劣... 海洋细粒沉积物中含有丰富的孢粉化石,不同的处理方法对孢粉富集程度的影响亦不同。为寻找简便而又环保的孢粉处理方法,满足我局地勘和科研项目大批量孢粉研究需要,开展氢氟酸重液浮选法和酸碱过筛法两种不同方法在富集孢粉方面的优劣对比研究,选用了10个南海陆坡沉积岩心的样品进行分组对比研究。结果显示,酸碱过筛法得到的孢粉丰度、去除有机质、分散性和制片效果明显优于氢氟酸重液浮选法,更有利于孢粉的鉴定。但是,氢氟酸重液浮选法得到的孢粉纹饰的清晰度和去除无机质方面更优于酸碱过筛法。 展开更多
关键词 南海细粒沉积物 孢粉 氢氟酸浮选 酸碱过筛
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三重四级杆液质联用法快速测定全血样中9种抗凝血类灭鼠剂 被引量:7
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作者 贾玉珠 蔡伟鹏 +3 位作者 陈丽惠 白艳艳 骆和东 朱宝平 《中国卫生检验杂志》 CAS 2016年第22期3196-3200,共5页
目的建立三重四级杆液质联用法,同时测定鼠药中毒患者血液样品中9种常见抗凝血类灭鼠剂(杀鼠醚、杀鼠灵、敌鼠钠盐、氯敌鼠、溴敌隆、大隆、杀它仗、鼠得克、氯杀鼠灵)。方法试样用乙腈提取,高速冷冻离心,过0.2μm滤膜,直接经液相色谱... 目的建立三重四级杆液质联用法,同时测定鼠药中毒患者血液样品中9种常见抗凝血类灭鼠剂(杀鼠醚、杀鼠灵、敌鼠钠盐、氯敌鼠、溴敌隆、大隆、杀它仗、鼠得克、氯杀鼠灵)。方法试样用乙腈提取,高速冷冻离心,过0.2μm滤膜,直接经液相色谱柱分离,在MRM模式下以三重四级杆质谱检测器测定血液中9种灭鼠剂。结果本方法中,9种抗凝血类灭鼠剂的空白血样加标回收率为75.3%~109.8%,相对标准偏差为2.6%~10.8%,在0.05μg/L^500.00μg/L的浓度内,相关系数>0.998,检出限为0.004μg/L^1.200μg/L,定量限为0.014μg/L^4.000μg/L。结论该法简单、快速、灵敏度高、定性确证和定量准确,可同时对血液中溴敌隆、大隆、氯敌鼠、杀鼠灵等9种灭鼠剂进行定性确证和定量测定,满足突发中毒事件快速应急检测的要求。 展开更多
关键词 四级杆质联用 中毒 全血 抗凝血类灭鼠剂
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三重四极杆液质联用法测定花生中4种黄曲霉毒素的研究 被引量:5
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作者 贾玉珠 贾沁一 +2 位作者 周娜 白艳艳 牛建军 《中国卫生检验杂志》 北大核心 2013年第10期2224-2226,共3页
目的建立LC/MS/MS法同时检测花生中黄曲霉毒素B1、B2、G1和G2的方法。方法粉碎后混匀的样品经70%甲醇提取,免疫亲和柱净化,在MRM模式下用LC/MS/MS法测定食品中黄曲霉毒素B1、B2、G1和G2含量。结果黄曲霉毒素B1、B2、G1和G2的加标回收率... 目的建立LC/MS/MS法同时检测花生中黄曲霉毒素B1、B2、G1和G2的方法。方法粉碎后混匀的样品经70%甲醇提取,免疫亲和柱净化,在MRM模式下用LC/MS/MS法测定食品中黄曲霉毒素B1、B2、G1和G2含量。结果黄曲霉毒素B1、B2、G1和G2的加标回收率77%~109%,相对标准偏差为3.2%~5.7%;在0.1 ng/ml~100 ng/ml浓度范围内具有很好线性,相关系数大于0.999;方法检出限小于0.08μg/kg、定量限小于0.3μg/kg。结论该法简单、快速、灵敏和特异性强,可同时对花生中黄曲霉毒素B1、G1、G2和B2进行定性确证和定量测定。 展开更多
关键词 免疫亲和柱 四极杆质联用 花生 黄曲霉毒素
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三重串联四级杆液质联用法测定人血浆中布洛芬浓度的不确定度评定 被引量:1
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作者 董晓茜 杨瑞 +3 位作者 唐思 张世良 刘君 夏素霞 《中国药物经济学》 2022年第2期122-124,128,共4页
目的评定三重串联四级杆液质联用法测定人血浆中布洛芬浓度的不确定度。方法对该实验测定方法全过程进行分析,建立评定不确定度的数学模型,确定影响不确定度的各个因素并进行评估,计算合成不确定度和扩展不确定度。结果置信概率P为95%时... 目的评定三重串联四级杆液质联用法测定人血浆中布洛芬浓度的不确定度。方法对该实验测定方法全过程进行分析,建立评定不确定度的数学模型,确定影响不确定度的各个因素并进行评估,计算合成不确定度和扩展不确定度。结果置信概率P为95%时,血浆中低(0.220 2μg/ml)、中(5.504μg/ml)、高(22.02μg/ml)浓度的布洛芬扩展不确定度分别为6.12μg/ml、11.80μg/ml、32.22μg/ml。结论本方法适用于三重串联四级杆液质联用法测定人血浆中布洛芬浓度的不确定度评定。 展开更多
关键词 布洛芬 血浆 串联四级杆质联用 不确定度
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火山灰的提取及测试技术 被引量:8
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作者 隋淑珍 刘嘉麒 +3 位作者 郭正府 Valerie A.HALL Chris S.M.TURNEY 王文远 《地学前缘》 EI CAS CSCD 2003年第1期111-116,共6页
同一次火山爆发产生的火山灰 ,能在广阔的区域内形成等时标志层 ,成为地层定年和对比的极有价值的工具。文中介绍了提取肉眼不可见火山灰的 4种方法 :烧失法、稀碱法、重液浮选法和酸化法 ,还介绍了火山玻璃的显微镜下识别技术及电子探... 同一次火山爆发产生的火山灰 ,能在广阔的区域内形成等时标志层 ,成为地层定年和对比的极有价值的工具。文中介绍了提取肉眼不可见火山灰的 4种方法 :烧失法、稀碱法、重液浮选法和酸化法 ,还介绍了火山玻璃的显微镜下识别技术及电子探针测试技术。 展开更多
关键词 火山灰 火山爆发 等时标志层 地层定年 烧失 稀碱 浮选 酸化 电子探针
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面膜中荧光增白剂的透皮吸收特性及对皮肤刺激性的实验研究 被引量:4
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作者 张虹艳 石晓峰 +3 位作者 王小乔 刘兴国 刘亚鹏 李赟 《日用化学工业》 CAS 北大核心 2022年第3期322-327,共6页
为了研究含脂溶性荧光增白剂(FWAs)面膜的透皮吸收特性及其对皮肤刺激性,采用改良的Franz透皮扩散池,以离体雄性大鼠腹部皮肤为模型,通过高效液相色谱-三重四极杆液质联用法测定接收液中5种吡唑啉型荧光增白剂的含量,计算其不同透皮时... 为了研究含脂溶性荧光增白剂(FWAs)面膜的透皮吸收特性及其对皮肤刺激性,采用改良的Franz透皮扩散池,以离体雄性大鼠腹部皮肤为模型,通过高效液相色谱-三重四极杆液质联用法测定接收液中5种吡唑啉型荧光增白剂的含量,计算其不同透皮时间段的累计渗透量,并对试验终期皮肤中FWAs的贮留量进行检测;按《化妆品安全技术规范》(2015年版)中皮肤刺激性实验要求,采用家兔进行皮肤刺激性试验。结果显示,5种脂溶性FWAs呈现良好的线性关系,相关系数(r;)均大于0.999,检出限为0.5~10.0 pg,定量限为2.0~30.0 pg,平均回收率和相对标准偏差分别为95.2%~102.1%和1.8%~4.2%。面膜中的脂溶性荧光增白剂C.I.162有较强的透皮能力可以进入皮下,在0~36 h内透皮扩散符合零级动力学方程;而C.I.135、C.I.185、C.I.367、C.I.368四种FWAs短期内均被皮肤吸收而未透过皮肤。结果提示,脂溶性FWAs较易迁移到皮肤的角质层或皮下,对哺乳动物皮肤没有刺激作用。 展开更多
关键词 面膜 荧光增白剂 透皮吸收 皮肤刺激性 高效相色谱-三四极杆质联用
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Reconstructing bubble profiles from gas-liquid two-phase flow data using agglomerative hierarchical clustering method 被引量:2
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作者 WU Dong-ling SONG Yan-po +1 位作者 PENG Xiao-qi GAO Dong-bo 《Journal of Central South University》 SCIE EI CAS CSCD 2019年第8期2056-2067,共12页
The knowledge of bubble profiles in gas-liquid two-phase flows is crucial for analyzing the kinetic processes such as heat and mass transfer, and this knowledge is contained in field data obtained by surface-resolved ... The knowledge of bubble profiles in gas-liquid two-phase flows is crucial for analyzing the kinetic processes such as heat and mass transfer, and this knowledge is contained in field data obtained by surface-resolved computational fluid dynamics (CFD) simulations. To obtain this information, an efficient bubble profile reconstruction method based on an improved agglomerative hierarchical clustering (AHC) algorithm is proposed in this paper. The reconstruction method is featured by the implementations of a binary space division preprocessing, which aims to reduce the computational complexity, an adaptive linkage criterion, which guarantees the applicability of the AHC algorithm when dealing with datasets involving either non-uniform or distorted grids, and a stepwise execution strategy, which enables the separation of attached bubbles. To illustrate and verify this method, it was applied to dealing with 3 datasets, 2 of them with pre-specified spherical bubbles and the other obtained by a surface-resolved CFD simulation. Application results indicate that the proposed method is effective even when the data include some non-uniform and distortion. 展开更多
关键词 bubble profile reconstruction gas-liquid two-phase flow clustering method surface-resolved computational fluid dynamics (CFD) distorted bubble shape
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Liquid Chromatography-tandem Mass Spectrometry for Analysis of Acylcarnitines in Dried Blood Specimens Collected at Autopsy from Neonatal Intensive Care Unit 被引量:2
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作者 Wen-jun Tu Fang Dai +2 位作者 Xin-yu Wang Ying Li James Jian Ho 《Chinese Medical Sciences Journal》 CAS CSCD 2010年第2期109-114,共6页
Objective To investigate the feasibility of analyzing acylcarnitine in dry filter-paper blood spots by liquid chromatography-tandem mass spectrometry(LC-MS/MS) which could be applied to detect inborn errors of metabol... Objective To investigate the feasibility of analyzing acylcarnitine in dry filter-paper blood spots by liquid chromatography-tandem mass spectrometry(LC-MS/MS) which could be applied to detect inborn errors of metabolism in neonates.Methods We obtained filter-paper blood from 26 dead infants from a neonatal intensive care unit(NICU) between October 1,2008 and September 30,2009.Acylcarnitine and amino acid profiles were obtained with LC-MS/MS.Four infants underwent routine autopsy.The postmortem blood specimens were compared with newborn blood specimens,and with specimens obtained from older infants with metabolic disorders.Results Of all the 26 patients,5(19.2%) were diagnosed as having different kinds of diseases:3 with methylmalonic acidemia(the concentration of C3,and the ratio of C3/C16,C3/C2 increased),1 with maple syrup urine disease(the concentration of leucine and isoleucine increased),and 1 with isovaleric aci-demia(the concentration of C5 increased).Conclusions Postmortem metabolic test can explain infant deaths and provide estimates of deaths attributable to inborn errors of metabolism in NICU.LC-MS/MS is suitable for analysis of postmortem specimens and can be considered for routine application in NICU autopsy. 展开更多
关键词 tandem mass spectrometry inborn errors of metabolism neonatal intensive care unit AUTOPSY
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Optimization of DsbA Purification from Recombinant Escherichia coli Broth Using Box-Behnken Design Methodolog 被引量:1
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作者 LUO Man GUAN Yixin YAO Shanjing 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2013年第2期185-191,共7页
Disulfide bond formation protein A (DsbA) is one of the important helper proteins for folding in protein synthesis in vivo. In this study, purification of recombinant DsbA was investigated by examining four importan... Disulfide bond formation protein A (DsbA) is one of the important helper proteins for folding in protein synthesis in vivo. In this study, purification of recombinant DsbA was investigated by examining four important factors with Box-Behnken design method, a statistic-based design of experiments. The optimal operation conditions were obtained by adopting the effectiveness coefficient method on the multi-objective problem, which takes the protein recovery, purification efficiency and throughput of ion-exchange chromatography into account. After the optimization, protein recovery of 96.8% and purity higher than 95% DsbA was achieved, and the productivity was (377.9±1.7) mg soluble DsbA per liter broth. The purified protein was identified by peptide mass fingerprinting matching the record of gil2624856, a mutant of DsbA. The DsbA was preliminarily applied to the refolding of denatured lysozyme in vitro. 展开更多
关键词 disulfide bond formation protein A protein purification Box-Behnken experiment design response surface methodology multi-object programming
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Measurement of Ice Movement in Water Using Electrical Capacitance Tomography 被引量:2
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作者 JIANG Fan LIU Shi +1 位作者 LIU Jing WANG Xueyao 《Journal of Thermal Science》 SCIE EI CAS CSCD 2009年第1期8-12,共5页
The permafrost with the highest altitude and largest area in the mid and low latitude is located in the Qinghad-Tibet Plateau. As most frozen soils contain ice particles which are very sensitive to temperature and oth... The permafrost with the highest altitude and largest area in the mid and low latitude is located in the Qinghad-Tibet Plateau. As most frozen soils contain ice particles which are very sensitive to temperature and other external parameters, thus influencing the stability of the embankment in permafrost regions, it is very important to develop techniques to prevent damages to railway embankments due to thaw settlement. In this paper, the electrical capacitance sensors are designed to study the freezing front movement in a vessel and ice movement in water, which is the first step to apply the ECT system to the study of frozen soil. Two sensor arrangements are put into use. First, the traditional closed electrode sensors are put into use. In this arrangement, the electrodes are attached to the outside of the pipe or vessel, and the cross-sectional distribution of ice and water could be reconstructed from the capacitances measured. Also, the ice moving track at the cross section could be reflected thoroughly.Since the traditional closed electrode sensors can not meet the needs of measuring the ice freezing front move- ment, a new electrode sensors structure, that is, the unclosed electrode sensors are designed to satisfy the specific test of frozen soil. In this arrangement, several pairs of electrodes are arranged along the height of the vessel. A sudden decrease in the measured capacitance is observed when the freezing front advances past the electrodes.Therefore, according to the capacitance variation, the ice movement can be reflected. In summary, electrical capacitance tomography has the advantages of being non-intrusive. With different electrode sensor arrangement, ice movement and ice freezing front can be obtained. The electrical capacitance sensor system can be applied to investigate the complicated phenomena in frozen soil. 展开更多
关键词 Electrical Capacitance Tomography Ice-Water Interface Two-Phase Flows Frozen Soil
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Polymorphic Pb_(14)O_(8)I_(12) and Pb_(7)O_(4)I_(6) oxyhalides featuring unprecedented[O_(8)Pb_(14)]clusters with broad IR transparency
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作者 Jiahao Jiao Abudukadi Tudi +4 位作者 Min Zhang Wenbing Cai Junjie Li Zhihua Yang Shilie Pan 《Science China Materials》 SCIE EI CAS CSCD 2022年第3期773-779,共7页
Wide transmittance range is an essential factor for the design of infrared optical materials.Traditionally,the designs of mid-far infrared crystals have focused on oxygenfree systems of chalcogenides and pnictides.Nev... Wide transmittance range is an essential factor for the design of infrared optical materials.Traditionally,the designs of mid-far infrared crystals have focused on oxygenfree systems of chalcogenides and pnictides.Nevertheless,the introduction of elements with large atomic numbers,such as the lone-pair cation Pb^(2+) and halogen anion I^(-),based on the oxyhalides,can broaden the infrared transmittance range.Thus,two new polymorphs of Pb(Ⅱ)-containing oxyhalides,Pb_(14)O_(8)I_(12)(α-POI)and Pb_(7)O_(4)I_(6)(β-POI),are successfully synthesized via the high-temperature solution method.Interestingly,they crystallize in the same space group,P1,and present unprecedented[O_(8)Pb_(14)]clusters from the perspective of oxocentered[OPb_(4)]basic units.Remarkably,POI exhibits a quite wide transparent range(0.47-16.0μm),which enlightens the oxyhalides with prominent infrared optical properties.Additionally,the first principles calculations show that they have large birefringence(0.139 and 0.108 for α-and β-POI at 1064 nm,respectively),which makes POI promising infrared optical materials. 展开更多
关键词 POLYMORPHS OXYHALIDES far-infrared transparent window birefringence optical materials
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