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气相色谱/高分辨质谱联用测定环境样品中的二噁英和类二噁英多氯联苯 被引量:27
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作者 任曼 彭平安 +4 位作者 张素坤 邓芸芸 麦碧娴 盛国英 傅家谟 《分析化学》 SCIE EI CAS CSCD 北大核心 2007年第2期176-180,共5页
样品采用索氏抽提,抽提液依次经酸性硅胶床、多段混合硅胶柱和凝胶渗透色谱柱(GPC)净化后,用Florisil硅藻土柱分离出样品中的二噁英(PCDD/Fs)和类二噁英多氯联苯(dioxin-like PCBs),采用同位素稀释法和气相色谱/高分辨质谱联用仪(GC/HR... 样品采用索氏抽提,抽提液依次经酸性硅胶床、多段混合硅胶柱和凝胶渗透色谱柱(GPC)净化后,用Florisil硅藻土柱分离出样品中的二噁英(PCDD/Fs)和类二噁英多氯联苯(dioxin-like PCBs),采用同位素稀释法和气相色谱/高分辨质谱联用仪(GC/HRMS)测定了其中的17个2,3,7,8-氯取代二噁英类化合物和12个类二噁英多氯联苯。结果表明,用该法分析二噁英和多氯联苯标准溶液,平行4次的分析结果为:RSD(PCDD/Fs)<8.9%,RSD(PCBs)<11.4%;回收率可达60%-105%。PCDD/Fs和PCBs的检出限分别为0.1-0.8 pg/g和0.05-0.6 pg/g。应用本方法成功测定了沉积物、淤泥、土壤和飞灰中的二噁英和类二噁英多氯联苯,并计算出它们的毒性当量。 展开更多
关键词 二噁英 类二噁英多氯联苯 气相色谱/高分辨质谱 Florisil硅藻土柱 环境样品
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GC-MS内标法测定发酵食品中氨基甲酸乙酯的含量 被引量:9
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作者 李晓芹 金尉 袁小美 《中国调味品》 北大核心 2017年第6期135-138,共4页
建立了发酵食品中氨基甲酸乙酯含量的气相色谱-质谱测定方法。以氨基甲酸乙酯-D5为内标,经硅藻土柱富集净化,二氯甲烷洗脱,气相色谱-质谱仪选择离子模式测定。方法优化后,液体样品检出限为2μg/kg,定量限为5μg/kg;固体样品检出限为5μg... 建立了发酵食品中氨基甲酸乙酯含量的气相色谱-质谱测定方法。以氨基甲酸乙酯-D5为内标,经硅藻土柱富集净化,二氯甲烷洗脱,气相色谱-质谱仪选择离子模式测定。方法优化后,液体样品检出限为2μg/kg,定量限为5μg/kg;固体样品检出限为5μg/kg,定量限为15μg/kg,回收率为85%~115%,RSD<6.0。该方法简单、有效、稳定,可应用于多种发酵食品中氨基甲酸乙酯的实际检测分析。 展开更多
关键词 氨基甲酸乙酯 硅藻土柱 内标法 气相色谱-质谱法
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发酵乳中氨基甲酸乙酯的测定 被引量:4
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作者 袁小美 金尉 陈娟 《农产品加工(下)》 2017年第1期53-55,共3页
建立发酵乳中氨基甲酸乙酯含量测定的气相色谱质谱方法。发酵乳样品除蛋白后,取清液进行硅藻土柱富集净化,二氯甲烷洗脱,气相色谱-质谱仪选择离子模式测定。为保证回收率,以氨基甲酸乙酯-D5为内标。氨基甲酸乙酯在10~500μg/L范围内线... 建立发酵乳中氨基甲酸乙酯含量测定的气相色谱质谱方法。发酵乳样品除蛋白后,取清液进行硅藻土柱富集净化,二氯甲烷洗脱,气相色谱-质谱仪选择离子模式测定。为保证回收率,以氨基甲酸乙酯-D5为内标。氨基甲酸乙酯在10~500μg/L范围内线性关系良好,相关系数R2=0.999 9。按信噪比3∶1确定检出限为2μg/kg,信噪比10∶1确定定量限为5μg/kg。回收率在85%~109%,RSD<8.7。此方法可应用于发酵乳中氨基甲酸乙酯的测定。 展开更多
关键词 氨基甲酸乙酯 硅藻土柱 内标法 气相色谱质谱法 发酵乳
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猪肉中常见的9种蓄水类药物残留的快速筛查 被引量:2
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作者 陈树兵 余晓玲 +4 位作者 李双 方科益 余晓琴 韩超 王传现 《分析科学学报》 CAS CSCD 北大核心 2021年第2期188-192,共5页
本文将载体辅助液-液萃取技术和高分辨质谱联用,用于9种猪肉蓄水类药物残留的的检测筛查。与水溶性化合物多通过离子交换固相萃取小柱净化浓缩的传统方法相比较,建立的方法通过大孔硅藻土柱吸附水相提取液,并将上层乙腈作为洗脱液,在乙... 本文将载体辅助液-液萃取技术和高分辨质谱联用,用于9种猪肉蓄水类药物残留的的检测筛查。与水溶性化合物多通过离子交换固相萃取小柱净化浓缩的传统方法相比较,建立的方法通过大孔硅藻土柱吸附水相提取液,并将上层乙腈作为洗脱液,在乙腈逐级渗入替换掉水溶液的同时,实现了9种常见蓄水类药物的净化和浓缩过程。结果表明:本方法对猪肉基质具有较强的适用性,肾上腺素及其代谢物的线性范围为5.0~50.0 ng/mL,定量限为5.0μg/kg,其他待测物线性范围为0.5~5.0 ng/mL,定量限为0.5μg/kg。加标回收率在80.7%~103.1%之间,相对标准偏差低于10%。该方法对水溶性化合物兼容性强,灵敏度高,可用于猪肉中常见的9种蓄水类药物:肾上腺素及其代谢物4-羟基-3-甲氧基-扁桃酸和3,4-二羟基扁桃酸、异丙嗪、阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因的快速筛查。 展开更多
关键词 蓄水类药物 大孔硅藻土柱 四极杆/静电场轨道阱高分辨质谱
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Polyhydroxyl-aluminum pillaring improved adsorption capacities of Pb^(2+) and Cd^(2+) onto diatomite 被引量:5
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作者 朱健 王平 +1 位作者 雷明婧 张伟丽 《Journal of Central South University》 SCIE EI CAS 2014年第6期2359-2365,共7页
In order to greatly improve adsorption capacity, the diatomite was pillared by polyhydroxyl-aluminum.A series of adsorption tests were conducted to obtain the optimum condition for pillared diatomite synthesis. The sc... In order to greatly improve adsorption capacity, the diatomite was pillared by polyhydroxyl-aluminum.A series of adsorption tests were conducted to obtain the optimum condition for pillared diatomite synthesis. The scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), surface area and porosity analyzer and micro-electrophoresis were used to determine pore structure and surface property.The pillared diatomite attaining the optimal adsorption densities (qe) of Pb^2+ and Cd^2+ was synthesized with the following conditions: Addition of pillaring solution containing Al3+-oligomers with a concentration range of 0.1-0.2 mol/L to a suspension containing Na+-diatomite to obtain the required Al/diatomite ratio of 10 mmol/g; synthesis temperature of 80 ℃ for 120 min; aging at a temperature of 105 ℃ for 16 h. The adsorption capacities of Pb^2+ and Cd^2+ on pillared diatomite increase by 23.79% and 27.36% compared with natural diatomite, respectively. The surface property of pillared diatomite is more favorable for ion adsorption than natural diatomite. The result suggests that diatomite can be modified by pillaring with polyhydroxyl-aluminum to improve its adsorption properties greatly. 展开更多
关键词 DIATOMITE PILLARING polyhydroxyl-aluminum synthesis ADSORPTION Pb^2+ Cd^2+
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Valorization of natural diatomite mineral:Application to removal of anionic dye from aqueous solution in a batch and fixed-bed reactor 被引量:1
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作者 HADRI Mohamed EL MRABET Imane +4 位作者 CHAOUKI Zineb DRAOUI Khalid HAMDAOUI Mustapha DOUHRI Hikmat ZAITAN Hicham 《Journal of Central South University》 SCIE EI CAS CSCD 2022年第6期2084-2098,共15页
In this work,the efficiency of an adsorption process,in which Moroccan diatomite(ND)is used as a low-cost adsorbent to remove Congo red(CR)dye from contaminated waters in batch and column system,was examined.The influ... In this work,the efficiency of an adsorption process,in which Moroccan diatomite(ND)is used as a low-cost adsorbent to remove Congo red(CR)dye from contaminated waters in batch and column system,was examined.The influence of experimental conditions(pH,adsorbent dose and temperature)on the adsorption of CR onto the ND adsorbent was studied.A study of the adsorption kinetics for CR revealed that a pseudo-second-order model provided the best fit to the experimental kinetic data,and the equilibrium data were well described by the Langmuir isotherm model with an adsorption capacity of 6.07 mg/g using 15 g/L of ND,pH=6,contact time 3 h and 25℃.On the other hand,the ND regeneration tests were investigated and showed that the desorption reaches at least 50%when using ethanol as eluent.In addition,the adsorption process in a continuous mode was studied.Breakthrough curves were properly represented by the Yoon—Nelson model.Hence,the adsorption capacity of 5.71 mg/g was reached using 0.114 g of adsorbent,CR concentration of 6 mg/L and a flow of 1 mL/min under 25℃. 展开更多
关键词 Congo red ADSORPTION DIATOMITE fixed-bed column kinetic model
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