A rapid and sensitive method for quantitative determination of paclitaxel in rat plasmawas developed and validated by using ultra-performance liquid chromatography-tandemmass spectrometry (UPLC-MS/MS). Docetaxel was u...A rapid and sensitive method for quantitative determination of paclitaxel in rat plasmawas developed and validated by using ultra-performance liquid chromatography-tandemmass spectrometry (UPLC-MS/MS). Docetaxel was used as an internal standard anddiethyl ether was the liquideliquid extraction agent. Multiple reaction monitoring (MRM)mode via positive electrospray ionization (ESI) was applied to detect paclitaxel and IS at thetransitions m/z 854 / 286 and m/z 808.48 / 527.3, respectively. This method covered alinearity range from 5 to 5000 ng/ml, with the total run time of 3.0 min. In summary, a highthroughout UPLC-MS/MS method was successfully developed to measure paclitaxel in ratplasma and was applied to pharmacokinetic study after intravenous administration ofpaclitaxel.展开更多
Objective To determine ten B-vitamins in human milk by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Methods The pretreated human milk samples were adequately separated and quan...Objective To determine ten B-vitamins in human milk by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Methods The pretreated human milk samples were adequately separated and quantified within 11 min by UPLC-MS/MS with an Acquity UPLC HSS T3 column （2.1×100 mm, 1.8 μm）. The mobile phase was a gradient of 2.5 mmol/L ammonium formate aqueous solution and acetonitrile at a flow rate of 0.35 mL/min. Stable isotope internal standards were used in the analysis, to correct for the method variability, including matrix and ionization effects. The homogenized human milk samples were deproteinzed using methanol, unknown contaminants were extracted with diethyl ether and hydrophobic phase was discarded. The analytes were monitored via ESl＋ionization and detected in multiple reaction monitoring （MRM） with three acquisition functions. Results Calibration curves ranged from 0.5-160 ng/mL （thiamin, riboflavin, biotin, nicotinic acid, pyridoxine, pyridoxamine, pyridoxal）, and 2.5-800 ng/mL （pantothenic acid, FAD and nicotinamide） （R^2=0.990-0.999）. The relative recovery ranged from 80.1% to 120.2%; accuracy was determined to be 98.3% to 108.0%. Intra-day and inter-day variation were 3.4%-19.9% and 5.9%-18.1%, respectively. The limit of quantification （LOQ） for all vitamins was between 0.25 and 3 lag/L. Conclusion This method was successfully applied for simultaneous analysis of ten B-vitamins in human milk.展开更多
<p> <strong>Short Retraction Notice</strong> </p> <p> The paper does not meet the standards of "American Journal of Analytical Chemistry". The article has been retracted d...<p> <strong>Short Retraction Notice</strong> </p> <p> The paper does not meet the standards of "American Journal of Analytical Chemistry". The article has been retracted due to the conflicts of interests between all authors to straighten the academic record. Aim is to promote the circulation of scientific research by offering an ideal research publication platform with due consideration of internationally accepted standards on publication ethics. The Editorial Board would like to extend its sincere apologies for any inconvenience this retraction may have caused. The full retraction notice in PDF is preceding the original paper, which is marked "RETRACTED". </p>展开更多
目的:建立一种超高效液相色谱串联质谱法(Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS)法测定保健食品中非法添加乌地那非、氯地那非含量的检测方法。方法:色谱柱为Agilent ZORBX Eclipse Plus C_(18)柱...目的:建立一种超高效液相色谱串联质谱法(Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS)法测定保健食品中非法添加乌地那非、氯地那非含量的检测方法。方法:色谱柱为Agilent ZORBX Eclipse Plus C_(18)柱(50 mm×2.1 mm,1.8μm),以0.1%甲酸水溶液-乙腈(65∶35)为流动相梯度洗脱,流速0.2 mL·min^(-1),柱温35℃;采用电喷雾离子源正模式多反应监测模式,外标法定量。结果:溶剂空白无干扰,乌地那非、氯地那非在10~200 ng·mL^(-1)时线性关系良好,相关系数分别为0.9990和0.9997;乌地那非的平均回收率为90.0%~104.3%,相对标准偏差为0.2%~3.8%;氯地那非的平均回收率为92.3%~105.8%,相对标准偏差为0.3%~2.2%;两者方法检出限、定量限分别为25μg·kg^(-1)和50μg·kg^(-1)。结论:建立的方法准确、灵敏、专属性强,适用于保健食品中非法添加乌地那非、氯地那非的痕量分析。展开更多
建立QuEChERS-超高效液相色谱-串联质谱法测定土壤中戊唑醇、倍硫磷等农药残留,样品经乙腈振荡提取,加入盐包,振荡、离心,取上清液加入装有净化剂的15 m L萃取管中,振荡离心后取上清液过滤膜上机测定,质谱采用电喷雾电离、多反应检测模...建立QuEChERS-超高效液相色谱-串联质谱法测定土壤中戊唑醇、倍硫磷等农药残留,样品经乙腈振荡提取,加入盐包,振荡、离心,取上清液加入装有净化剂的15 m L萃取管中,振荡离心后取上清液过滤膜上机测定,质谱采用电喷雾电离、多反应检测模式(Multiple Reaction Monitoring,MRM)检测。检测结果显示,该方法线性良好,相关系数为0.992~0.999,在20、50、100μg·kg^(-1)3个水平浓度下加标回收率在80%~120%,相对标准偏差在20%以下。该方法简单、快捷、灵敏度高,满足检测要求。展开更多
基金This work was financially supported from the National Nature Science Foundation of China(No.81173008)from the National Basic Research Program of China(973 Program)No.2009CB930300+1 种基金from Project for Excellent Talents of Liaoning Province(No.LR20110028)from Program for New Century Excellent Talents in University(No.NCET-12-1015).
文摘A rapid and sensitive method for quantitative determination of paclitaxel in rat plasmawas developed and validated by using ultra-performance liquid chromatography-tandemmass spectrometry (UPLC-MS/MS). Docetaxel was used as an internal standard anddiethyl ether was the liquideliquid extraction agent. Multiple reaction monitoring (MRM)mode via positive electrospray ionization (ESI) was applied to detect paclitaxel and IS at thetransitions m/z 854 / 286 and m/z 808.48 / 527.3, respectively. This method covered alinearity range from 5 to 5000 ng/ml, with the total run time of 3.0 min. In summary, a highthroughout UPLC-MS/MS method was successfully developed to measure paclitaxel in ratplasma and was applied to pharmacokinetic study after intravenous administration ofpaclitaxel.
基金supported by the National High Technology Research and Development Program of China(863 Program)(No.2010AA023004)
文摘Objective To determine ten B-vitamins in human milk by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Methods The pretreated human milk samples were adequately separated and quantified within 11 min by UPLC-MS/MS with an Acquity UPLC HSS T3 column （2.1×100 mm, 1.8 μm）. The mobile phase was a gradient of 2.5 mmol/L ammonium formate aqueous solution and acetonitrile at a flow rate of 0.35 mL/min. Stable isotope internal standards were used in the analysis, to correct for the method variability, including matrix and ionization effects. The homogenized human milk samples were deproteinzed using methanol, unknown contaminants were extracted with diethyl ether and hydrophobic phase was discarded. The analytes were monitored via ESl＋ionization and detected in multiple reaction monitoring （MRM） with three acquisition functions. Results Calibration curves ranged from 0.5-160 ng/mL （thiamin, riboflavin, biotin, nicotinic acid, pyridoxine, pyridoxamine, pyridoxal）, and 2.5-800 ng/mL （pantothenic acid, FAD and nicotinamide） （R^2=0.990-0.999）. The relative recovery ranged from 80.1% to 120.2%; accuracy was determined to be 98.3% to 108.0%. Intra-day and inter-day variation were 3.4%-19.9% and 5.9%-18.1%, respectively. The limit of quantification （LOQ） for all vitamins was between 0.25 and 3 lag/L. Conclusion This method was successfully applied for simultaneous analysis of ten B-vitamins in human milk.
文摘<p> <strong>Short Retraction Notice</strong> </p> <p> The paper does not meet the standards of "American Journal of Analytical Chemistry". The article has been retracted due to the conflicts of interests between all authors to straighten the academic record. Aim is to promote the circulation of scientific research by offering an ideal research publication platform with due consideration of internationally accepted standards on publication ethics. The Editorial Board would like to extend its sincere apologies for any inconvenience this retraction may have caused. The full retraction notice in PDF is preceding the original paper, which is marked "RETRACTED". </p>
文摘目的:建立一种超高效液相色谱串联质谱法(Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS)法测定保健食品中非法添加乌地那非、氯地那非含量的检测方法。方法:色谱柱为Agilent ZORBX Eclipse Plus C_(18)柱(50 mm×2.1 mm,1.8μm),以0.1%甲酸水溶液-乙腈(65∶35)为流动相梯度洗脱,流速0.2 mL·min^(-1),柱温35℃;采用电喷雾离子源正模式多反应监测模式,外标法定量。结果:溶剂空白无干扰,乌地那非、氯地那非在10~200 ng·mL^(-1)时线性关系良好,相关系数分别为0.9990和0.9997;乌地那非的平均回收率为90.0%~104.3%,相对标准偏差为0.2%~3.8%;氯地那非的平均回收率为92.3%~105.8%,相对标准偏差为0.3%~2.2%;两者方法检出限、定量限分别为25μg·kg^(-1)和50μg·kg^(-1)。结论:建立的方法准确、灵敏、专属性强,适用于保健食品中非法添加乌地那非、氯地那非的痕量分析。
文摘建立QuEChERS-超高效液相色谱-串联质谱法测定土壤中戊唑醇、倍硫磷等农药残留,样品经乙腈振荡提取,加入盐包,振荡、离心,取上清液加入装有净化剂的15 m L萃取管中,振荡离心后取上清液过滤膜上机测定,质谱采用电喷雾电离、多反应检测模式(Multiple Reaction Monitoring,MRM)检测。检测结果显示,该方法线性良好,相关系数为0.992~0.999,在20、50、100μg·kg^(-1)3个水平浓度下加标回收率在80%~120%,相对标准偏差在20%以下。该方法简单、快捷、灵敏度高,满足检测要求。
