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中药复方“清开灵”注射液中胆酸类物质的液相色谱/质谱/质谱分析 被引量:14
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作者 刘国文 刘密新 +2 位作者 吴筑平 杨成对 罗国安 《分析化学》 SCIE EI CAS CSCD 北大核心 2001年第6期621-624,共4页
采用液相色谱/质谱/质谱法,通过保留时间、分子量和二级质谱的信息对复方“清开灵”注射液中的胆酸、去氧胆酸和鹅去氧腿酸进行了定性;建立了内标法对复方中相对含量较大的胆酸的定量分析方法;结果表明胆酸在875 ng/L-1... 采用液相色谱/质谱/质谱法,通过保留时间、分子量和二级质谱的信息对复方“清开灵”注射液中的胆酸、去氧胆酸和鹅去氧腿酸进行了定性;建立了内标法对复方中相对含量较大的胆酸的定量分析方法;结果表明胆酸在875 ng/L-140μg/L范围内线性良好,线性相关系数R2=0.9999;RSD=2.4%。该方法样品处理简单,选择性好,灵敏度高。对中药的质量控制具有重要的意义。 展开更多
关键词 胆酸 去氧胆酸 鹅去氧胆酸 中药 液相色谱-质谱/谱分析 清开灵注射液 定量分析
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原油与油砂生物标志化合物特征差异对比及正构烷烃散焦作用对其定量的影响
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作者 李玮 《中国科技期刊数据库 工业A》 2024年第6期0018-0023,共6页
基于南堡凹陷原油与油砂样品,探讨了原油和油砂样品饱和烃生物标志化合物的特征及差异。针对原油/油砂样品色谱-质谱分析数据可能存在的错误,利用色谱-质谱(GC-MS)技术和色谱-质谱质谱(GC-MSMS)技术对相同油砂与原油样品设计了三组对比... 基于南堡凹陷原油与油砂样品,探讨了原油和油砂样品饱和烃生物标志化合物的特征及差异。针对原油/油砂样品色谱-质谱分析数据可能存在的错误,利用色谱-质谱(GC-MS)技术和色谱-质谱质谱(GC-MSMS)技术对相同油砂与原油样品设计了三组对比实验。第一组为原始的GC-MS实验,第二组为重复的GC-MS实验,第三组为相同样品的GC-MSMS实验。南堡凹陷1号和2号构造带中浅层原油均为成熟原油,其生烃母质形成于弱还原的淡水沉积环境,以低等水生生物为主,高等植物输入次之。本文对比实验证实:正构烷烃散焦作用对第一组实验的生物标志化合物定量造成严重误差,并且对甾烷类的影响较萜烷类更显著。由于挥发作用,油砂样品普遍缺少低碳数烃类。得到三点启示:①建议优先采集原油样品,慎重使用含油级别较低的油砂样品。②利用GC-MS数据前,应对数据的有效性进行分析,排除误差的影响。③GC-MS结果可以代替GC-MSMS结果,但是建议选择适当原油/油砂样品进行GC-MSMS平行实验,利用平行实验结果对GC-MS结果进行校正。 展开更多
关键词 原油 油砂 色谱-谱分析 色谱-质谱谱分析 生物标志化合物 南堡凹陷
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Product Identification and Mass Spectrometric Analysis of n-Butane and i-Butane Pyrolysis at Low Pressure 被引量:1
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作者 张义军 苑文浩 +3 位作者 蔡江淮 张李东 齐飞 李玉阳 《Chinese Journal of Chemical Physics》 SCIE CAS CSCD 2013年第2期151-156,I0003,共7页
The pyrolysis of n-butane and i-butane at low pressure was investigated from 823-1823 K in an electrically heated flow reactor using synchrotron vacuum ultraviolet photoionization mass spectrometry. More than 20 speci... The pyrolysis of n-butane and i-butane at low pressure was investigated from 823-1823 K in an electrically heated flow reactor using synchrotron vacuum ultraviolet photoionization mass spectrometry. More than 20 species, especially several radicals and isomers, were detected and identified from the measurements of photoionization efficiency (PIE) spectra. Based on the mass spectrometric analysis, the characteristics of n-butane and i-butane pyrolysis were discussed, which provided experimental evidences for the discussion of decomposition pathways of butane isomers. It is concluded that the isomeric structures of n-butane and i-butane have strong influence on their main decomposition pathways, and lead to dramatic differences in their mass spectra and PIE spectra such as the different dominant products and isomeric structures of butene products. Furthermore, compared with n-butane,i-butane can produce strong signals of benzene at low temperature in its pyrolysis due to the enhanced formation of benzene precursors like propargyl and C4 species, which provides experimental clues to explain the higher sooting tendencies of iso-alkanes than n-alkanes. 展开更多
关键词 N-BUTANE /-Butane Flow reactor pyrolysis Synchrotron vacuum ultravioletphotoionization mass spectrometry Product identification Mass spectrometric analysis
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Diethylstilbestrol in Fish Tissue Determined Through Subcritical Fluid Extraction and with GC-MS 被引量:1
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作者 QIAO Qinghui SHI Nianrong +3 位作者 FENG Xiaomei LU Jie HAN Yuqian XUE Changhu 《Journal of Ocean University of China》 SCIE CAS 2016年第3期489-494,共6页
As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more effici... As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples. 展开更多
关键词 subcritical R134a extraction DIETHYLSTILBESTROL GC-MS determination fish tissue
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某些炸药在CI源中的行为——TNT、RDX、PETN、HMX和特屈儿的正负CI谱 被引量:5
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作者 徐建中 彭耀珊 汪聪慧 《刑事技术》 1994年第5期1-4,共4页
本文采用质谱仪的正、负化学源及MS/MS方式检测炸药残留物,方法简单、快速、灵敏度高,样品用量少,而且可用于混和物的直接分析。
关键词 炸药残留物 化学源(CI) 质谱-质谱分析
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Characterization of impurities in the bulk drug lisinopril by liquid chromatography/ion trap spectrometry
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作者 Pei-xi ZHU Dan-hua WANG +1 位作者 Cui-rong SUN Zhi-quan SHEN 《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》 SCIE CAS CSCD 2008年第5期385-390,共6页
Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry (HPLC/MS) with a simple and sensitive method suitable for HPLC/MSn ana... Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry (HPLC/MS) with a simple and sensitive method suitable for HPLC/MSn analysis. The fragmentation behavior of lisinopfil and the impurities was investigated, and two unknown impurities were elucidated as 2-(6-amino- l-(l-carboxyethylamino)- l-oxohexan-2-ylamino)-4-phenylbutanoic acid and 6-amino-2-(l-carboxy-3-phenylpropylamino)-hexanoic acid on the basis of the multi-stage mass spectrometry and exact mass evidence, The proposed structures of the two unknown impurities were further confirmed by nuclear magnetic resonance (NMR) experiments after preparative isolation. 展开更多
关键词 LISINOPRIL IMPURITIES High-performance liquid chromatography (HPLC) Multi-stage mass spectrometry (MS^n)
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Rapid Analysis of Nicotine in Mushrooms Using QuEChERS Extraction and Liquid Chromatography Tandem Mass Spectrometry
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作者 A. Santilio R. Dommarco 《Journal of Food Science and Engineering》 2011年第1期27-34,共8页
A procedure based on the QuEChERS methodology and Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) is described, for the determination of Nicotine in mushrooms. QuEChERS methodology was used to determine Ni... A procedure based on the QuEChERS methodology and Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) is described, for the determination of Nicotine in mushrooms. QuEChERS methodology was used to determine Nicotine in dried and fresh mushrooms under basic conditions with primary secondary amino sorbent (PSA) clean up. The chromatography was performed on C 18 reversed phase column using a gradient of acetonitrile and ammonium formiate lmM pH = 3.4 as mobile phase at a flow rate of 0.3 mL min^-1. Nicotine was determined by using Nicotine-d3 as internal standard. Limit of quantification (LOQ) was 0.01 mg kg^-1 for both fresh and dried mushrooms. Calibration curve was linear over the concentration range of 0.01-2.3 mg mL^-1, with r2 〉 0.99. As for recoveries in dried mushrooms, spiking levels of 0.32 mg kg^-1 and 2 mg kg^-1 were considered whereas for the fresh mushrooms the recoveries were determined at 0.036 mg kg^-1 and 0.36 mg kg^-1. Satisfactory results were obtained for both matrices and the recoveries proved to range from 105% to 135%, with a standard deviation in the range 17-20. The method was applied to the analysis of Nicotine to assess the levels of nicotine in fresh and dried mushrooms. 展开更多
关键词 QUECHERS NICOTINE MUSHROOMS PESTICIDES RESIDUES liquid chromatography tandem mass spectrometry (LC/MS/MS)
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Comprehensive profiling of lysine acetylome in Staphylococcus aureus 被引量:2
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作者 ZHANG Yi WU ZhiXiang +5 位作者 WAN XueLian LIU Ping ZHANG JiBao YE Yang ZHAO YingMing TAN MinJia 《Science China Chemistry》 SCIE EI CAS 2014年第5期732-738,共7页
The Gram-positive bacterium Staphylococcus aureus(S.aureus)is a wide spread common opportunistic pathogen that causes a wide variety of infectious diseases,from benign skin infections to life-threatening diseases such... The Gram-positive bacterium Staphylococcus aureus(S.aureus)is a wide spread common opportunistic pathogen that causes a wide variety of infectious diseases,from benign skin infections to life-threatening diseases such as the methicillin-resistant Staphylococcus aureus(MRSA)infection.Although emerging evidence suggests that lysine acetylation may play critical roles in bacterial physiology,the atlas of acetylome in S.aureus has not been studied.To comprehensively profile protein lysine acetylation in S.aureus,we used an integrated approach that combined immune affinity peptide enrichment using anti-lysine acetylation antibody,high-pH HPLC fractionation,and HPLC/mass spectrometry analysis.This study led to the identification of 1361 non-redundant acetylation sites on 412 proteins found in a search of S.aureus protein database extracted from the Swiss-Prot database.We further performed bioinformatic analysis to characterize this modification,including gene ontology annotation,protein-protein interaction,and domain analysis of the acetylation sites.We found that the acetylated proteins were enriched in multiple biological pathways,such as ribosomal function and energy metabolism.Our data provides a rich source for functional studies of lysine acetylation in S.aureus. 展开更多
关键词 PROTEOMICS post-translational modification ACETYLATION Staphylococcus aureus
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