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
The comparison of solid phase extraction（SPE） for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry （UPLC/...The comparison of solid phase extraction（SPE） for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry （UPLC/MS/MS） and multivariate analysis.Several adsorbing materials of SPE（C18,NH2,SAX and OASIS） were investigated.It was found that the C18 and OASIS cartridges can not only speed up the purification process,but also simplify the SPE operation.A UPLC/MS/MS was used for the determination of polyphenols in tobacco samples after purification.All analytes were separated and determined in 2min.The limit of detection was 0.05 ng/mL.Cluster analysis（CA） and principal component analysis（PCA） were used for the analysis of 4 varieties（flue-cured tobacco,oriental tobacco,sun-cured tobacco and burley） in order to interpret the effect of planting and machining process on the concentration of polyphenols.The different types of tobacco samples could be easily clustered by CA.PCA on the chemical composition of tobacco resulted in two principal components（PCs） that take 84.2% of the total variance.The PCA and CA indicate that the polyphenols can be used for distinguishing tobacco types.展开更多
该研究建立了沙棘药材及食品制品中10种真菌毒素的分析方法,对其真菌毒素的污染情况进行分析。首先选取黄曲霉毒素、赭曲霉毒素、玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇等10种真菌毒素的混合对照品溶液作为对照,并对沙棘药材及其食品制品进...该研究建立了沙棘药材及食品制品中10种真菌毒素的分析方法,对其真菌毒素的污染情况进行分析。首先选取黄曲霉毒素、赭曲霉毒素、玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇等10种真菌毒素的混合对照品溶液作为对照,并对沙棘药材及其食品制品进行制备;其次基于超高效液相色谱-串联质谱法(ultra-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)对沙棘药材及食品制品中10种真菌毒素做定量方法学考察并对其含量进行测定;最后对真菌毒素的污染情况进行分析评价。分析结果确定了最佳分析条件,且方法学考察结果表明10种真菌毒素建立的线性关系良好(r>0.99),方法重复性,供试品专属性、稳定性,仪器精密度均良好;10种真菌毒素在沙棘药材、沙棘食品制品固体和沙棘食品制品液体3种基质中的平均加样回收率分别为90.31%~109.4%、87.86%~107.8%、85.61%~109.1%;RSD分别为0.22%~10%、0.75%~13%、0.84%~8.5%。说明该研究基于UPLC-MS/MS技术建立的10种真菌毒素限度的同时测定方法检测速度快、基质干扰较少、灵敏度高、结果准确,适用于沙棘药材及其食品制品中的10种真菌毒素的限度检查。展开更多
文摘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.
基金Supported by the Foundation of State Tabacco Monopoly Bureau(China) in Research Project(No.110200902008)
文摘The comparison of solid phase extraction（SPE） for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry （UPLC/MS/MS） and multivariate analysis.Several adsorbing materials of SPE（C18,NH2,SAX and OASIS） were investigated.It was found that the C18 and OASIS cartridges can not only speed up the purification process,but also simplify the SPE operation.A UPLC/MS/MS was used for the determination of polyphenols in tobacco samples after purification.All analytes were separated and determined in 2min.The limit of detection was 0.05 ng/mL.Cluster analysis（CA） and principal component analysis（PCA） were used for the analysis of 4 varieties（flue-cured tobacco,oriental tobacco,sun-cured tobacco and burley） in order to interpret the effect of planting and machining process on the concentration of polyphenols.The different types of tobacco samples could be easily clustered by CA.PCA on the chemical composition of tobacco resulted in two principal components（PCs） that take 84.2% of the total variance.The PCA and CA indicate that the polyphenols can be used for distinguishing tobacco types.
文摘该研究建立了沙棘药材及食品制品中10种真菌毒素的分析方法,对其真菌毒素的污染情况进行分析。首先选取黄曲霉毒素、赭曲霉毒素、玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇等10种真菌毒素的混合对照品溶液作为对照,并对沙棘药材及其食品制品进行制备;其次基于超高效液相色谱-串联质谱法(ultra-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)对沙棘药材及食品制品中10种真菌毒素做定量方法学考察并对其含量进行测定;最后对真菌毒素的污染情况进行分析评价。分析结果确定了最佳分析条件,且方法学考察结果表明10种真菌毒素建立的线性关系良好(r>0.99),方法重复性,供试品专属性、稳定性,仪器精密度均良好;10种真菌毒素在沙棘药材、沙棘食品制品固体和沙棘食品制品液体3种基质中的平均加样回收率分别为90.31%~109.4%、87.86%~107.8%、85.61%~109.1%;RSD分别为0.22%~10%、0.75%~13%、0.84%~8.5%。说明该研究基于UPLC-MS/MS技术建立的10种真菌毒素限度的同时测定方法检测速度快、基质干扰较少、灵敏度高、结果准确,适用于沙棘药材及其食品制品中的10种真菌毒素的限度检查。
