A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with flucona...A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with fluconazole as an Internal Standard and directed to protein precipitation and drug extraction. An aliquot of 1 μl was injected into the chromatographic system and separated by the Acquity BEH C18 column at a flow rate of 0.30 ml/min in a gradient mobile phase consisting of acetonitrile, Ultrapure water (UPW), methanol and formic acid. Voriconazole was detected by a Triple Quadrupole Detector (TQD) operating on Multiple Reaction Monitoring (MRM) and a positive ion mode Electrospray ionization (ESI) Q1 mass: 350.1 m/z, Q3 mass: 281.1 m/z. Method linearity of the calibration curve (0.10 - 8.00 μg/ml) indicated a correlation coefficient r ≥ 0.99. The intra and inter-assay accuracy was within 85% - 115% and the intra and inter-assay precision was ≤5.76%. Voriconazole recovery percentage was between 97.69 - 119.62%. The method was successively applied in routine voriconazole TDM.展开更多
An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracte...An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics.展开更多
基于食品基质中松仁过敏原Pin k 2建立了一种超高效液相色谱-串联质谱法。将松仁经过研磨、脱脂、浸提、酶解后经Easy-nLC 1000-QExactive高分辨质谱仪进行分离分析,结合Uniprot蛋白数据库以及ProteinPilotTM软件对质谱图进行数据处理,...基于食品基质中松仁过敏原Pin k 2建立了一种超高效液相色谱-串联质谱法。将松仁经过研磨、脱脂、浸提、酶解后经Easy-nLC 1000-QExactive高分辨质谱仪进行分离分析,结合Uniprot蛋白数据库以及ProteinPilotTM软件对质谱图进行数据处理,经BLAST验证特异性,最终筛选3条松仁特异性肽段。方法学验证结果表明,方法在0.001~50mg/mL范围内线性关系良好,定量限为1mg/kg;在饼干、巧克力和饮料3种空白基质中的平均回收率为88.50%~107.57%,相对标准偏差不高于6.08%,基质效应为89.77%~96.13%。该方法具有灵敏度高、特异性好的优势,可应用于饼干、巧克力、饮料等食品样品中松仁过敏原的检测,为我国食品标签真实性检验及食品中隐性过敏原的检测提供技术支持。展开更多
采用十八烷基三氯硅烷(octadecyltrichlorosilane,OTS)与N-[3-(三甲氧基硅基)丙基]乙二胺(N-[3-(trimethoxysilyl)propyl]ethylenediamine,ATS)改性三聚氰胺海绵(melamine sponge,MeS)制备得到2种新型弹性多孔硅烷化MeS(OTS@MeS和ATS@M...采用十八烷基三氯硅烷(octadecyltrichlorosilane,OTS)与N-[3-(三甲氧基硅基)丙基]乙二胺(N-[3-(trimethoxysilyl)propyl]ethylenediamine,ATS)改性三聚氰胺海绵(melamine sponge,MeS)制备得到2种新型弹性多孔硅烷化MeS(OTS@MeS和ATS@MeS)净化材料,将其用于改良QuEChERS(quick,easy,cheap,effective,rugged and safe)基质净化过程,通过溶液自发浸润和物理挤压过程即可快速、高效分离干扰基质,结合超高效液相色谱-串联质谱技术建立了同时测定猪肉中49种抗生素多残留的分析方法。样品用1.0%乙酸-乙腈溶液提取并用2.0 g Na_(2)SO_(4)和0.5 g NaCl盐析,离心后取1 mL上清液复配使用OTS@MeS与ATS@MeS净化,随后使用Agilent ZORBAX Eclipse Plus C_(18)色谱柱,以甲醇溶液和含有0.1%甲酸、5 mmol/L乙酸铵的甲醇-水溶液(5∶95,V/V)为流动相进行梯度洗脱,采用电喷雾电离源、正离子多反应监测模式进行定性定量分析。结果表明:49种抗生素的相关系数均大于0.999,基质效应为-13.5%~10.9%,检出限在0.1~10μg/kg之间,定量限在0.3~30.3μg/kg之间;利用该方法在低、中、高3个加标水平下进行回收率实验,回收率范围为65.0%~112.7%,日内和日间相对标准偏差分别为0.3%~11.8%和2.4%~18.4%。该方法样品前处理过程简单、快捷、灵敏度高、准确性好,可用于猪肉中49种抗生素多残留的高效快速检测。展开更多
The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Gi...The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.展开更多
建立了直接进样-超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)同时测定地下水中2,4-二氯苯氧乙酸(2,4-D)、乐果、涕灭威、克百威、敌敌畏、莠去津、甲基对硫磷、马拉硫磷、五氯酚和毒死蜱等10种有机农药方法。水样经0.22μm滤膜过滤...建立了直接进样-超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)同时测定地下水中2,4-二氯苯氧乙酸(2,4-D)、乐果、涕灭威、克百威、敌敌畏、莠去津、甲基对硫磷、马拉硫磷、五氯酚和毒死蜱等10种有机农药方法。水样经0.22μm滤膜过滤,以甲醇和水为流动相,梯度洗脱,流速为0.4 m L·min^(-1),进样量为10μL,采用电喷雾正、负离子电离模式,多反应监测(MRM)检测,经内标法定量分析。10种有机农药的质量浓度在0.2~20μg·L^(-1)的范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.995,方法检出限为0.01~0.05μg·L^(-1),3个加标水平样品的平均回收率为82.3~116%,相对标准偏差为0.66~21.5%(n=6)。该方法操作简单高效,所需水样体积少且灵敏度高,满足地下水质量标准I类水限值,能够适应实际大批量地下水样品中10种有机农药的快速分析。展开更多
文摘A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with fluconazole as an Internal Standard and directed to protein precipitation and drug extraction. An aliquot of 1 μl was injected into the chromatographic system and separated by the Acquity BEH C18 column at a flow rate of 0.30 ml/min in a gradient mobile phase consisting of acetonitrile, Ultrapure water (UPW), methanol and formic acid. Voriconazole was detected by a Triple Quadrupole Detector (TQD) operating on Multiple Reaction Monitoring (MRM) and a positive ion mode Electrospray ionization (ESI) Q1 mass: 350.1 m/z, Q3 mass: 281.1 m/z. Method linearity of the calibration curve (0.10 - 8.00 μg/ml) indicated a correlation coefficient r ≥ 0.99. The intra and inter-assay accuracy was within 85% - 115% and the intra and inter-assay precision was ≤5.76%. Voriconazole recovery percentage was between 97.69 - 119.62%. The method was successively applied in routine voriconazole TDM.
文摘An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics.
文摘基于食品基质中松仁过敏原Pin k 2建立了一种超高效液相色谱-串联质谱法。将松仁经过研磨、脱脂、浸提、酶解后经Easy-nLC 1000-QExactive高分辨质谱仪进行分离分析,结合Uniprot蛋白数据库以及ProteinPilotTM软件对质谱图进行数据处理,经BLAST验证特异性,最终筛选3条松仁特异性肽段。方法学验证结果表明,方法在0.001~50mg/mL范围内线性关系良好,定量限为1mg/kg;在饼干、巧克力和饮料3种空白基质中的平均回收率为88.50%~107.57%,相对标准偏差不高于6.08%,基质效应为89.77%~96.13%。该方法具有灵敏度高、特异性好的优势,可应用于饼干、巧克力、饮料等食品样品中松仁过敏原的检测,为我国食品标签真实性检验及食品中隐性过敏原的检测提供技术支持。
文摘采用十八烷基三氯硅烷(octadecyltrichlorosilane,OTS)与N-[3-(三甲氧基硅基)丙基]乙二胺(N-[3-(trimethoxysilyl)propyl]ethylenediamine,ATS)改性三聚氰胺海绵(melamine sponge,MeS)制备得到2种新型弹性多孔硅烷化MeS(OTS@MeS和ATS@MeS)净化材料,将其用于改良QuEChERS(quick,easy,cheap,effective,rugged and safe)基质净化过程,通过溶液自发浸润和物理挤压过程即可快速、高效分离干扰基质,结合超高效液相色谱-串联质谱技术建立了同时测定猪肉中49种抗生素多残留的分析方法。样品用1.0%乙酸-乙腈溶液提取并用2.0 g Na_(2)SO_(4)和0.5 g NaCl盐析,离心后取1 mL上清液复配使用OTS@MeS与ATS@MeS净化,随后使用Agilent ZORBAX Eclipse Plus C_(18)色谱柱,以甲醇溶液和含有0.1%甲酸、5 mmol/L乙酸铵的甲醇-水溶液(5∶95,V/V)为流动相进行梯度洗脱,采用电喷雾电离源、正离子多反应监测模式进行定性定量分析。结果表明:49种抗生素的相关系数均大于0.999,基质效应为-13.5%~10.9%,检出限在0.1~10μg/kg之间,定量限在0.3~30.3μg/kg之间;利用该方法在低、中、高3个加标水平下进行回收率实验,回收率范围为65.0%~112.7%,日内和日间相对标准偏差分别为0.3%~11.8%和2.4%~18.4%。该方法样品前处理过程简单、快捷、灵敏度高、准确性好,可用于猪肉中49种抗生素多残留的高效快速检测。
文摘The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.
文摘建立了直接进样-超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)同时测定地下水中2,4-二氯苯氧乙酸(2,4-D)、乐果、涕灭威、克百威、敌敌畏、莠去津、甲基对硫磷、马拉硫磷、五氯酚和毒死蜱等10种有机农药方法。水样经0.22μm滤膜过滤,以甲醇和水为流动相,梯度洗脱,流速为0.4 m L·min^(-1),进样量为10μL,采用电喷雾正、负离子电离模式,多反应监测(MRM)检测,经内标法定量分析。10种有机农药的质量浓度在0.2~20μg·L^(-1)的范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.995,方法检出限为0.01~0.05μg·L^(-1),3个加标水平样品的平均回收率为82.3~116%,相对标准偏差为0.66~21.5%(n=6)。该方法操作简单高效,所需水样体积少且灵敏度高,满足地下水质量标准I类水限值,能够适应实际大批量地下水样品中10种有机农药的快速分析。
