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汽车玻璃用功能膜中有机物的气相色谱-质谱测定方法
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作者 王颖杰 赵文涛 李飞 《玻璃》 2022年第3期49-55,共7页
介绍了汽车玻璃用功能膜中有机物的气相色谱-质谱测定方法。明确了使用的气相色谱-质谱仪中各部分的参数设定,质谱仪性能的确认以及所需的热脱附仪、烘箱、充气泵、真空泵、气袋、吸附管等各种辅助设备与耗材的要求,介绍了实验过程中须... 介绍了汽车玻璃用功能膜中有机物的气相色谱-质谱测定方法。明确了使用的气相色谱-质谱仪中各部分的参数设定,质谱仪性能的确认以及所需的热脱附仪、烘箱、充气泵、真空泵、气袋、吸附管等各种辅助设备与耗材的要求,介绍了实验过程中须注意事宜。通过实验分析出常用汽车功能膜中对人体有毒有害的有机物种类,从而为定量分析打下基础。 展开更多
关键词 汽车玻璃用功能膜 气相色谱-质谱分析方法 袋子采样法 有机物定性分析
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运用顶空固相微萃取技术分析宣威火腿中的挥发性化合物 被引量:23
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作者 要萍 马长伟 +1 位作者 周珊 黄骏雄 《食品与发酵工业》 CAS CSCD 北大核心 2003年第10期1-5,共5页
采用固相微萃取结合气相色谱 /质谱分析方法对宣威火腿中的挥发性化合物进行了提取和分析。试验结果表明 ,固相微萃取的时间和温度影响提取挥发性化合物的效果 ,试验选取 60℃、60min为提取条件 ,萃取物经气谱 /质谱分析 ,共鉴定出 72... 采用固相微萃取结合气相色谱 /质谱分析方法对宣威火腿中的挥发性化合物进行了提取和分析。试验结果表明 ,固相微萃取的时间和温度影响提取挥发性化合物的效果 ,试验选取 60℃、60min为提取条件 ,萃取物经气谱 /质谱分析 ,共鉴定出 72种化合物 ,其中烃类 2 8种、醛类 7种、醇类 4种、酸类 10种、酯类 5种、酮类 3种、杂环化合物 14种、酚类 1种。 展开更多
关键词 宣威火腿 顶空固相微萃取技术 挥发性化合物 提取 气相色谱/质谱分析方法
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固相萃取/LC-MS/MS法检测动物源性食品中的金刚烷胺 被引量:31
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作者 云环 张朝晖 +1 位作者 罗生亮 张杉 《现代仪器》 2009年第6期42-45,共4页
建立测定动物源性食品中金刚烷胺的固相萃取/液相色谱一电喷雾串联质谱分析方法。以甲醇-1%三氯乙酸(50+50,v/v)作提取溶剂,采用超声波辅助溶剂萃取法萃取动物源性食品,萃取液用Waters Oasis MCX固相萃取柱进行净化浓缩。以ThermoHypers... 建立测定动物源性食品中金刚烷胺的固相萃取/液相色谱一电喷雾串联质谱分析方法。以甲醇-1%三氯乙酸(50+50,v/v)作提取溶剂,采用超声波辅助溶剂萃取法萃取动物源性食品,萃取液用Waters Oasis MCX固相萃取柱进行净化浓缩。以ThermoHypersil Gold C_(18)色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。对流动相组分和流动相添加剂对质谱的离子化效率进行考察,在1.0~50.0 ng/mL范围内线性关系良好(r?0.99)。样品在5.0 μg/k,10.0μg/k和20.0 μ g/kg添加水平的回收率为75.9%~108.5%,相对标准偏差小于8.0%;方法的检出限为5.0μg/kg。本方法具有很高的灵敏度和准确度,能够满足动物源性食品中的金刚烷胺残留量的快速、高灵敏检测分析。 展开更多
关键词 固相萃取柱 LC-MS/MS 检测分析 动物源性食品 金刚烷胺 质谱分析方法 相对标准偏差 流动相添加剂 电喷雾电离 正离子模式 串联谱仪 超声波辅助 液相色谱 线性关系 添加水平 提取溶剂 溶剂革取 测定 准确度 相组分
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A highly sensitive SPE-liquid/liquid extraction-RPLC analytical method for the determination of 6β-hydroxycortisol and cortisol in cancer patients' urine 被引量:3
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作者 Zhang Hong Fang Yu Li Ying Liang Aibin 《Journal of Medical Colleges of PLA(China)》 CAS 2010年第2期75-83,共9页
A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods: After SPE column purification and liquid-l... A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods: After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy (recovery from urine), repeatability (within-day and between-day precision), specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results: The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion: This new analytical method facilitates such individualized medical treatments. 展开更多
关键词 Solid phase extraction (SPE) Liquid/liquid extraction Reversed-phase high performance liquid chromatography (RPLC) CYP3A 6β-hydroxycortisol/cortisol Cancer
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Science Letters:Volatile constituents in the flowers of Elsholtzia argyi and their varia-tion:a possible utilization of plant resources after phytoremediation 被引量:3
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作者 彭红云 杨肖娥 《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》 SCIE CAS CSCD 2005年第2期91-95,共5页
Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was use... Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was used to investigate the volatiles of the flowers from Elsholtzia argyi (PFE1: Purple Flower Elsholtzia) and their variation (WFE: White Flower Elsholtzia),naturally growing in Pb/Zn mined area, and Elsholtzia argyi (PFE2: Purple Flower Elsholtzia), naturally growing in Jiuxi uncontaminated agriculture soil. Seventeen compounds constituting 86.88% of total essential oils were identified in PFE1, with 2,6-octadienoic acid,3,7-dimethyl-methyl ester being the main constituent (63.30%). Sixteen compounds accounting for 95.32% of total essential oils were identified in WFE, with caryophyllene being the main component (55.02%). Compared to PFE1, PFE2 contained lower level of 2,6-octadienoic acid,3,7-dimethyl-methyl ester (31.76%), which was the main constituent in the total essential oils of PFE2. Caryophyllene is the main ingredient of flavor. Elsholtzia ketone was identified in all the three Elsholtzia plants. It can be concluded that the selected Elsholtzia argyi plants can be exploited on their versatile uses as fragrances and antiseptics due to the perfume ingredient and antibacterial components existing in their essential oils. 展开更多
关键词 Elsholtzia argyi Essential oils GC/MS PHYTOREMEDIATION
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气相色谱-质谱法同时测定饲料中三聚氰胺和盐酸克伦特罗 被引量:2
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作者 王立君 吴银良 +1 位作者 杨挺 皇甫伟国 《畜牧与兽医》 北大核心 2010年第10期38-41,共4页
建立了同时测定饲料中三聚氰胺和盐酸克伦特罗的固相萃取-气相色谱-质谱分析方法。饲料样品用乙腈和50 mmol/L稀盐酸提取,然后用乙酸乙酯液液萃取净化,水相经PCX固相萃取小柱净化后用含1%三甲基氯硅烷的BSTFA衍生,采用选择离子模式进行... 建立了同时测定饲料中三聚氰胺和盐酸克伦特罗的固相萃取-气相色谱-质谱分析方法。饲料样品用乙腈和50 mmol/L稀盐酸提取,然后用乙酸乙酯液液萃取净化,水相经PCX固相萃取小柱净化后用含1%三甲基氯硅烷的BSTFA衍生,采用选择离子模式进行测定,三聚氰胺衍生物选择离子为213,285,327,342,盐酸克伦特罗衍生物选择离子为86,212,262,277,外标法定量,三聚氰胺和盐酸克伦特罗检出限分别为0.6μg/kg和2.4μg/kg。在添加浓度10~200μg/kg范围内,饲料中三聚氰胺和盐酸克伦特罗的回收率分别为81.3%~92.0%和70.8%~82.2%,批内RSD分别为2.6%~4.5%和2.7%~5.2%,批间RSD分别为3.8%~7.0%和5.4%~6.1%。衍生物的峰面积与样品浓度在0.01~0.50mg/L范围内呈良好的线性关系,线性回归系数均大于0.999。 展开更多
关键词 气相色谱 谱法 同时测定 饲料 三聚氰胺衍生物 盐酸克伦特罗 选择离子 固相萃取 质谱分析方法 线性回归系数 三甲基氯硅烷 乙酸乙酯 样品浓度 线性关系 添加浓度 萃取净化 子模式 柱净化 外标法 酸提取
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Adsorption and Transfer Properties for Toluene and pDichlorobenzene in Dense CO_2/Silica Gel Packed Bed System by Moment Method and Time-Domain Analysis
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作者 杨晓宁 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2003年第3期280-288,共9页
Based on chromatographic theory, the moment method and the time-domain fitting analysis were applied to measure and evaluate the adsorption equilibrium constant and mass transfer properties (axial dispersion coefficie... Based on chromatographic theory, the moment method and the time-domain fitting analysis were applied to measure and evaluate the adsorption equilibrium constant and mass transfer properties (axial dispersion coefficient and effective intra-particle diffusivity) for toluene and p-dichlorobenzene on silica gel adsorbent in the subcritical and supercritical CO2. An apparatus based on supercritical fluid chromatography was established and the experiments were performed at temperatures of 298.15-318.15 K and pressures of 7.5-17.8 MPa. The two methods have been compared. The results show that for the systems studied here the moment method can give reasonable values for both adsorption equilibrium constant and mass transfer properties, but the time-domain analysis only can obtain the adsorption equilibrium constant. The dependence of adsorption equilibrium constant and mass transfer properties on temperature and pressure was investigated. 展开更多
关键词 supercritical CO2 ADSORPTION CHROMATOGRAPHY moment method time-domain analysis
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LC-MS/MS法测定Beagle犬血浆中米拉贝隆缓释片的药动学特性 被引量:1
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作者 乔晓芳 杨利娟 +1 位作者 杨艳丽 张胜华 《临床医学》 CAS 2016年第5期104-107,共4页
目的建立Beagle犬血浆中米拉贝隆浓度测定的液相色谱串联质谱(LC-MS/MS)分析方法,研究米拉贝隆缓释片在犬体内的药动学特征。方法选取8只Beagle犬,雌雄各半,分成两组,每组4只,双交叉试验设计进行单剂量给药,分别给予50 mg受试制剂与参... 目的建立Beagle犬血浆中米拉贝隆浓度测定的液相色谱串联质谱(LC-MS/MS)分析方法,研究米拉贝隆缓释片在犬体内的药动学特征。方法选取8只Beagle犬,雌雄各半,分成两组,每组4只,双交叉试验设计进行单剂量给药,分别给予50 mg受试制剂与参比制剂,采集不同时间血浆样品,采用LC-MS/MS分析方法测定Beagle犬体内的血药浓度并计算主要药动学参数。结果与米拉贝隆缓释片市售品(商品名:Myrbetriq)相比,米拉贝隆缓释片自制品的Cmax值为市售品相应参数的132.29%(几何均值为112.67%),相对生物利用度为106.37%(几何均值为100.45%)。结论米拉贝隆缓释片自制品与市售品的药代动力学参数之间比较差异未见统计学意义,提示自制品与市售品的药代动力学行为无显著差异。 展开更多
关键词 液相色谱串联质谱分析方法 米拉贝隆缓释片 药动学
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Direct visualization of the charge transfer in conjugated polymers 被引量:1
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作者 LI Yan LI YuanZuo +1 位作者 DONG Bin YANG ZhiLin 《Science China(Physics,Mechanics & Astronomy)》 SCIE EI CAS 2011年第6期1119-1123,共5页
Ion-induced charge-transfer states in conjugated polyelectrolytes were experimentally investigated by Justin M.Hodgkiss and his co-workers [J Am Chem Soc,2009,131(25):8913].In this work,charged and neutral conjugated ... Ion-induced charge-transfer states in conjugated polyelectrolytes were experimentally investigated by Justin M.Hodgkiss and his co-workers [J Am Chem Soc,2009,131(25):8913].In this work,charged and neutral conjugated polyelectrolytes were further studied with quantum chemistry methods.The calculation result shows that the absorption spectra are roughly in visible and ultraviolet light regions,and the two absorption peaks are located in the wavelength span 300-400 nm for charged polyelectrolytes.However,in neutral conjugated polyelectrolytes,the peaks of the absorption spectra showed a blue shift compared with those of the charged polyelectrolytes.Charge transfer (CT) properties of the studied compounds were also investigated with both the three-dimensional real-space analysis method of transition and charge difference densities,and the two-dimensional real-space analysis method of transition density matrices based on the simulated absorption spectra.The calculation results revealed the charge transfer in conjugated polyelectrolytes on the excitation states. 展开更多
关键词 conjugated polyelectrolytes charger transfer charge difference density
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Kinetically controlled, high-yield, direct synthesis of [Au_(25)(SePh)_(18)]^-TOA^+
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作者 SONG YongBo CAO TianTian +3 位作者 DENG HuiJuan ZHU XiuYi LI Peng ZHU ManZhou 《Science China Chemistry》 SCIE EI CAS 2014年第9期1218-1224,共7页
In this article, we present a facile, direct, synthetic approach of preparing monodisperse [Au2s(SePh)ls]- nanoclusters in high yield. In this synthetic approach, two-phase Brust-Schiffrin method is used. Both PhSeH... In this article, we present a facile, direct, synthetic approach of preparing monodisperse [Au2s(SePh)ls]- nanoclusters in high yield. In this synthetic approach, two-phase Brust-Schiffrin method is used. Both PhSeH and NaBH4 should be added drop-wise to the solution of Au (III) at the same time. The formula and molecular purity of [Au25(SePh)ls] TOA+ clusters are characterized by MALDI-TOF mass spectrometry, NMR and TGA analysis. Furthermore, some critical parameters to obtain pure [Au25(SePh)18]-TOA+ are identified, including the NaBH4-to-Au ratio, the selenolate-to-Au ratio and the temperature. The facile, direct, high yield synthetic method can be widely applied in the theoretical research of Au clusters protected by selenol. 展开更多
关键词 selenophenol Au cluster Au2s(SePh)18 kinetically controlled atomic precision
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