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chzhbin金虫 (职业作家)
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建立并验证生物样品中TS IIA的灵敏、特异、可靠、线性范围广的检测方法。采用乙醚液-液萃取(diethyl ether-induced liquid-liquid extraction)提取生物样品中的TS IIA和内标氯雷他定(loratadine)，采用液相色谱-串联质谱方法检测。离子源为电喷雾离子化源（electro-spray ionization, ESI）；检测方式为正离子检测；扫描方式采用选择反应监测（SRM），用于定量分析的离子反应分别为m/z 295→249(TS IIA)和m/z 383→266（氯雷他定）。色谱分析柱为Hypersil BDS C18柱(2.1 mm×50 mm,5 m)；流动相为甲醇-水（90:10，v/v）(水中含1%甲酸)；流速为300 L/min；每个样品的分析时间为2 min。分析方法的定量下限为1.0 ngmL，各生物样品中TS IIA的线性相关程度良好（r2均大于0.99）。以质控样品计算该分析方法的批内精密度RSD在1.3% ~ 13.6%范围内，批间精密度RSD在1.0% ~ 10.9%范围内；方法的准确度在90.5% ~ 112.1%之间；方法的提取回收率在血浆中为60.2% ~ 67.3%，在肝匀浆中为68.6% ~ 71.4%，在尿、胆汁、粪匀浆中为50.7% ~ 67.5%，在HBSS、肠灌流液、肝微粒体体系中为37.3% ~ 49.6%。该分析方法经验证结果满意，样品处理及检测过程较已报道的方法简单、快速，可满足TS IIA临床前药代动力学研究的要求。 目的 方法 结果 结论 将这段摘要翻译成英文，目的，方法，结果，结论四项。 有谁能够把上面的液相色谱-串联质谱的参数列出来啊 [ Last edited by chzhbin on 2010-3-18 at 20:51 ] |
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zp5602
木虫 (小有名气)
- 应助: 0 (幼儿园)
- 金币: 2782.9
- 散金: 52
- 帖子: 173
- 在线: 231.2小时
- 虫号: 941754
- 注册: 2010-01-13
- 性别: GG
- 专业: 交叉学科中的光学问题
chzhbin(金币+30):很感激您 不过还有点不太规范 呵呵 有些语法错误 2010-03-18 18:07
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花了我好长时间，我不是这个专业的，早点给我金币啊 目的：Establish and validate a sensitive, specific and reliable test method with a wide linearity of TSIIA in the biological sample. 方法：Diethyl ether-induced liquid-liquid extraction is used to extract the TSIIA and loratadine in the biological sample and we use Liquid chromatograph-mass spectrometer to detect them. The ion source is electro-spray ionization (ESI). The detecting method employs positive ions and the scanning mode is SRM. The ions used for quantitative analysis are m/z 295→249(TS IIA) and m/z 383→266 respectively. Chromatograph column is Hypersil BDS C18 column (2.1 mm×50 mm,5 m) and the mobile phase is methanol-water (90:10, V/V) (1% methanol in the water). The flow velocity is 300 Hypersil BDS column (2.1 mm×50 mm, 5 mL in every biological sample TSL/min) and the analysis time for every sample is 2 min. The quantitative lower limit of the analysis method is 1.0 ngu and the correlation of linearity of IIA is good (all r2 bigger than 0.99). 结果：The RSD of accurate density within the group of this method calculated by the quality controlled sample is between 1.3%~13.6% and the RSD of accurate density beyond the group is between 1.0%~10.9%. The accuracy of is method is between 90.5%~112.1%. The recovery rate of extraction is 60.2%~67.3% in plasma and 68.6%~71.4% in the liver homogenate and 50.7% ~ 67.5% in the urine, bile and feces homogenate and 37.3% ~ 49.6% in the HBSS, intestines instilled liquid and lover particle systems. 结论：The validated results prove to be satisfactory. The treatment of the sample and testing process are more simple and faster than the previous reported method and can satisfy the demand the research of clinical pharmacokinetics. |
2楼2010-03-18 09:53:20