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毛细管电泳等离子体原子发射光谱测定人血浆中游离钙离子的含量 被引量:3
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作者 朱平川 徐祥书 +2 位作者 肖艳 杨坤国 邓必阳 《分析化学》 SCIE EI CAS CSCD 北大核心 2008年第11期1555-1558,共4页
毛细管电泳-电感耦合等离子体原子发射光谱联用技术应用于人体血浆中钙元素的形态分析,对游离钙离子进行了定位表征与定量分析。在电泳缓冲溶液为30 mmol/L Tris-HCl(pH=7.4)及电泳电压为20 kV的条件下,得到人体血浆中钙的主要形态有8... 毛细管电泳-电感耦合等离子体原子发射光谱联用技术应用于人体血浆中钙元素的形态分析,对游离钙离子进行了定位表征与定量分析。在电泳缓冲溶液为30 mmol/L Tris-HCl(pH=7.4)及电泳电压为20 kV的条件下,得到人体血浆中钙的主要形态有8种,其中一种为游离钙离子,迁移时间的相对偏差小于2%(n=10),血浆中游离钙离子的含量为42.2 mg/L,该测定方法RSD小于5%。采用以上联用技术测得血浆样品中游离钙离子回收率为94.8%-104%;方法检出限为25μg/L。 展开更多
关键词 毛细管电泳 电感耦合等离子体原子发射光谱 血浆 形态分析
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A rapid and sensitive liquid chromatography-tandem mass spectrometric assay for duloxetine in human plasma:Its pharmacokinetic application 被引量:4
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作者 Ramakrishna Gajula Rambabu Maddela +2 位作者 Vasu Babu Ravi Jaswanth Kumar Inamadugu Nageswara Rao Pilli 《Journal of Pharmaceutical Analysis》 SCIE CAS 2013年第1期36-44,共9页
This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope (duloxetine ds) was us... This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope (duloxetine ds) was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer (83:17, v/v) as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear (r2≥0.99) over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode (MRM) was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies. 展开更多
关键词 Duloxetine in humanplasma Solid-phase extraction(SPE) Liquidchromatography-tandem mass spectro-metry Method validation Pharmacokinetic studies
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LC-MS/MS Method for the Quantitation of Cefotetan in Human Plasma and Its Application to Pharmacokinetic Study
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作者 SHI Meiyun YIN Lei +8 位作者 CAI Lanlan WANG Can LIU Xidong ZHAO Sen SUN Yantong FAWCETT J. Paul ZHAO Limei YANG Yan GU Jingkai 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2014年第6期900-904,共5页
A rapid and sensitive liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the de- termination of cefotetan in human plasma was developed and validated. After the protein precipitation of sample with ... A rapid and sensitive liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the de- termination of cefotetan in human plasma was developed and validated. After the protein precipitation of sample with acetonitrile, the analyte and internal standard(IS), tramadol, were separated on a Zorbax XDB C8 column using ace- tonitrile/1%(volume fraction) formic acid(volume ratio 35:65, pH=2.5) as mobile phase at a flow rate of 1.0 mL/min with a 1 : 1 split. The detection was performed by electrospray ionization with positive ion mode, followed by multiple reaction monitoring of the transitions for cefotetan at m/z 576.3→460.2(quantifier) and m/z 576.3→432.2(qualifier) and for IS at m/z 264.1→58.1. Cefotetan and IS were eluted at 1.86 and 1.87 rain, respectively. The assay was linear over the concentration range of 0.1-100 gg/mL for 20 μL of human plasma only with intra- and inter-day preci- sions(expressed as the relative standard deviation) of less than 6.62% and accuracies(as relative error) of +1.31%. The method was applied to the pharmacokinetic study of a l-h intravenous infusion of 1.0 g of cefotetan disodium for human volunteers(n=6). 展开更多
关键词 CEFOTETAN Liquid chromatography-tandem mass spectrometry(LC-MS/MS) PHARMACOKINETICS humanplasma
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