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
Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ul...Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for simultaneous determination of fluticasone propionate and salmeterol xinofoate in human plasma. Following a simple SPE sample extraction in 96-well plate format, chromatography was performed on a Waters ACQUITY UPLC BEH C 18 column （1.7 μm, 50 min×2.1 mm） with mobile phase consisting of 100% MeOH and 0.1% NH4OH in water on a gradient program at flow rate of 0.5 mL/min. Detection of analytes and internal standards was accomplished using multiple reaction monitoring （MRM） of precursor〉product ion pairs of m/z 501.4〉313.2 （fluticasone propionate）, 506.4〉293.3 （fluticasone propionate-d5）, 416.4〉232.1 （salmeterol xinofoate） and 419.3〉235.2 （salmeterol-d3）. The assay range was 2.50-500 pg/mL for both analytes, and a 1/x2 weighted linear regression model was used. The inter-assay accuracy and precision of the method were within ±8.6%. The recoveries from 0.30 mL of plasma were greater than 51.0% and 54.6% for fluticasone propionate and salmeterol, respectively, and the results were consistent across low, middle and high concentration levels. The method was validated following FDA, EMA and CFDA （China Food and Drug Administration）＇s guidance on bioanalysis and then successfully applied to support a clinical study in healthy Chinese subjects following inhaled administration of a single combination of fluticasone propionate/salmeterol （250 μg/50 μg）.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
目的建立定量测定大鼠血浆中顺式二苯乙烯苷[cis-2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(TSG)]与反式二苯乙烯苷(trans-TSG)血药浓度的UPLC-MS/MS方法,系统探究2种异构体在大鼠体内的药动学差异。方法将40只雄性SD大鼠随机分为...目的建立定量测定大鼠血浆中顺式二苯乙烯苷[cis-2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(TSG)]与反式二苯乙烯苷(trans-TSG)血药浓度的UPLC-MS/MS方法,系统探究2种异构体在大鼠体内的药动学差异。方法将40只雄性SD大鼠随机分为4组(每组10只),即cis-TSG ig给药组、cis-TSG尾iv给药组、trans-TSG ig给药组、transTSG尾iv给药组。ig组给药剂量为100 mg·kg^(-1),尾iv组给药剂量为10 mg·kg^(-1);于给药前(0 h)及给药后0.030、0.083、0.160、0.250、0.330、0.500、1.000、2.000、4.000、6.000、8.000、10.000、12.000、24.000 h,通过眼静脉丛采集血样。以虎杖苷为内标,测定上述2个成分在不同时间点的血药浓度;利用DAS 1.0软件计算药动学参数,分析其药动学行为差异。结果所建立的UPLC-MS/MS方法在专属性、稳定性、准确度与精密度方面均符合体内药物浓度测定的技术要求,且无明显基质效应、提取回收率稳定。药动学结果显示:①给药途径对暴露水平影响显著:2种成分经iv给药后的血药浓度-时间曲线下面积(AUC)、达峰浓度(C_(max))均显著高于ig给药,且达峰时间(t_(max))更短,提示iv给药可使药物直接、快速进入体循环;②异构体间暴露差异显著:无论是iv还是ig给药,cis-TSG的AUC、C_(max)均显著高于trans-TSG(P<0.05),cis-TSG的消除半衰期(t_(1/2))长于trans-TSG[iv(7.03 h vs 2.63 h)、ig(16.90 h vs 8.46 h)],提示2种异构体在吸收、代谢或分布过程中存在本质差异;③口服生物利用度较低:cis-TSG与trans-TSG的口服绝对生物利用度分别为28.46%、27.35%。结论cis-TSG与trans-TSG在大鼠体内的药动学行为存在显著差异,主要体现为cis-TSG的体内暴露水平更高、消除更缓慢;且2种成分的口服生物利用度均较低。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Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for simultaneous determination of fluticasone propionate and salmeterol xinofoate in human plasma. Following a simple SPE sample extraction in 96-well plate format, chromatography was performed on a Waters ACQUITY UPLC BEH C 18 column （1.7 μm, 50 min×2.1 mm） with mobile phase consisting of 100% MeOH and 0.1% NH4OH in water on a gradient program at flow rate of 0.5 mL/min. Detection of analytes and internal standards was accomplished using multiple reaction monitoring （MRM） of precursor〉product ion pairs of m/z 501.4〉313.2 （fluticasone propionate）, 506.4〉293.3 （fluticasone propionate-d5）, 416.4〉232.1 （salmeterol xinofoate） and 419.3〉235.2 （salmeterol-d3）. The assay range was 2.50-500 pg/mL for both analytes, and a 1/x2 weighted linear regression model was used. The inter-assay accuracy and precision of the method were within ±8.6%. The recoveries from 0.30 mL of plasma were greater than 51.0% and 54.6% for fluticasone propionate and salmeterol, respectively, and the results were consistent across low, middle and high concentration levels. The method was validated following FDA, EMA and CFDA （China Food and Drug Administration）＇s guidance on bioanalysis and then successfully applied to support a clinical study in healthy Chinese subjects following inhaled administration of a single combination of fluticasone propionate/salmeterol （250 μg/50 μg）.
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>
文摘目的建立定量测定大鼠血浆中顺式二苯乙烯苷[cis-2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(TSG)]与反式二苯乙烯苷(trans-TSG)血药浓度的UPLC-MS/MS方法,系统探究2种异构体在大鼠体内的药动学差异。方法将40只雄性SD大鼠随机分为4组(每组10只),即cis-TSG ig给药组、cis-TSG尾iv给药组、trans-TSG ig给药组、transTSG尾iv给药组。ig组给药剂量为100 mg·kg^(-1),尾iv组给药剂量为10 mg·kg^(-1);于给药前(0 h)及给药后0.030、0.083、0.160、0.250、0.330、0.500、1.000、2.000、4.000、6.000、8.000、10.000、12.000、24.000 h,通过眼静脉丛采集血样。以虎杖苷为内标,测定上述2个成分在不同时间点的血药浓度;利用DAS 1.0软件计算药动学参数,分析其药动学行为差异。结果所建立的UPLC-MS/MS方法在专属性、稳定性、准确度与精密度方面均符合体内药物浓度测定的技术要求,且无明显基质效应、提取回收率稳定。药动学结果显示:①给药途径对暴露水平影响显著:2种成分经iv给药后的血药浓度-时间曲线下面积(AUC)、达峰浓度(C_(max))均显著高于ig给药,且达峰时间(t_(max))更短,提示iv给药可使药物直接、快速进入体循环;②异构体间暴露差异显著:无论是iv还是ig给药,cis-TSG的AUC、C_(max)均显著高于trans-TSG(P<0.05),cis-TSG的消除半衰期(t_(1/2))长于trans-TSG[iv(7.03 h vs 2.63 h)、ig(16.90 h vs 8.46 h)],提示2种异构体在吸收、代谢或分布过程中存在本质差异;③口服生物利用度较低:cis-TSG与trans-TSG的口服绝对生物利用度分别为28.46%、27.35%。结论cis-TSG与trans-TSG在大鼠体内的药动学行为存在显著差异,主要体现为cis-TSG的体内暴露水平更高、消除更缓慢;且2种成分的口服生物利用度均较低。
