目的：建立超高效液相色谱-质谱法（UPLC—ESI-Q-TOF／MS）同时测定保健食品中24种违禁精神药品的检测方法。方法：样品经甲醇超声振荡提取，0．22μm滤膜过滤后进样，分析。采用Agilent Eclipse Plus C18柱分离，流动相：0．1％甲酸（...目的：建立超高效液相色谱-质谱法（UPLC—ESI-Q-TOF／MS）同时测定保健食品中24种违禁精神药品的检测方法。方法：样品经甲醇超声振荡提取，0．22μm滤膜过滤后进样，分析。采用Agilent Eclipse Plus C18柱分离，流动相：0．1％甲酸（A），0．1％甲酸-甲醇（B），梯度洗脱；采用电喷雾离子源、正、负离子模式、利用Q-TOF的一、二级精密质量数进行定性，一级准分子离子峰定量检测。结果：24种精神药品在线性范围内线性关系良好，相关系数均大于0．990；检出限在1．56～218．2ng·ml^-1之间；回收率为64．60％～99．33％；相对标准偏差均小于7％。结论：该方法选择性强、灵敏度高、处理方法简单，可用于保健品中违禁镇静安神类化学药品的筛查与测定。展开更多
[目的]阐明远志中的化学成分。[方法]采用超高效液相色谱-电喷雾离子化-四级杆飞行时间串联质谱(UPLC/ESI-Q-TOF MS)法分析远志中的化学成分,采用Masslynx V 4.1软件,通过分析准分子离子和二级碎片离子信息,并进一步根据标准品的色谱保...[目的]阐明远志中的化学成分。[方法]采用超高效液相色谱-电喷雾离子化-四级杆飞行时间串联质谱(UPLC/ESI-Q-TOF MS)法分析远志中的化学成分,采用Masslynx V 4.1软件,通过分析准分子离子和二级碎片离子信息,并进一步根据标准品的色谱保留时间和质谱裂解规律,鉴定远志中的化学成分。[结果]鉴定了远志中29个化学成分,主要为口山酮、低聚糖酯、皂苷类成分。[结论]总结归纳了远志药材中主要化学成分的质谱裂解规律,阐明了远志中的主要化学成分。展开更多
Objective To identify the coumarins constituents in Cnidium monnieri and classify ten samples into three groups and this helpful chemical information could be used for the further pharmacological and clinical study on...Objective To identify the coumarins constituents in Cnidium monnieri and classify ten samples into three groups and this helpful chemical information could be used for the further pharmacological and clinical study on C. monnieri. Methods Qualitative analysis of coumarins in C. monnieri was detected by UHPLC-ESI-Q-TOF/MS. Quadrupole TOF/MS in either full scan mode or extracted ion mode was used for the qualitative analysis of the constituents. Relative peak area of each component was used for the hierarchical cluster analysis. Results According to UHPLC-ESI-QTOF-MS data, chemical structures of 28 coumarins in the fruits of C. monnieri were identified, including 19 simple coumarins, seven linear coumarins, and two angular coumarins. Among these constituents, ten coumarins were firstly identified in C. monnieri. In addition, hierarchical cluster analysis suggested that C. monnieri from different regions could be classified into four groups, and this clustering was correlated to the distribution significantly, Xuzhou could be regarded as the genuine producing area. Conclusion UHPLC-ESI-Q-TOF-MS is a viable method for qualitative analysis and quality evaluation of coumarins from the fruit of C. monnieri. Coumarins in C. monnieri exists intra-species variance, which indicates significant meaning for the quality control and choice of famous region drug for C. monnieri in the clinic medication.展开更多
文摘目的：建立超高效液相色谱-质谱法（UPLC—ESI-Q-TOF／MS）同时测定保健食品中24种违禁精神药品的检测方法。方法：样品经甲醇超声振荡提取，0．22μm滤膜过滤后进样，分析。采用Agilent Eclipse Plus C18柱分离，流动相：0．1％甲酸（A），0．1％甲酸-甲醇（B），梯度洗脱；采用电喷雾离子源、正、负离子模式、利用Q-TOF的一、二级精密质量数进行定性，一级准分子离子峰定量检测。结果：24种精神药品在线性范围内线性关系良好，相关系数均大于0．990；检出限在1．56～218．2ng·ml^-1之间；回收率为64．60％～99．33％；相对标准偏差均小于7％。结论：该方法选择性强、灵敏度高、处理方法简单，可用于保健品中违禁镇静安神类化学药品的筛查与测定。
文摘[目的]阐明远志中的化学成分。[方法]采用超高效液相色谱-电喷雾离子化-四级杆飞行时间串联质谱(UPLC/ESI-Q-TOF MS)法分析远志中的化学成分,采用Masslynx V 4.1软件,通过分析准分子离子和二级碎片离子信息,并进一步根据标准品的色谱保留时间和质谱裂解规律,鉴定远志中的化学成分。[结果]鉴定了远志中29个化学成分,主要为口山酮、低聚糖酯、皂苷类成分。[结论]总结归纳了远志药材中主要化学成分的质谱裂解规律,阐明了远志中的主要化学成分。
基金National Natural Science Foundation of China(No.81202865)
文摘Objective To identify the coumarins constituents in Cnidium monnieri and classify ten samples into three groups and this helpful chemical information could be used for the further pharmacological and clinical study on C. monnieri. Methods Qualitative analysis of coumarins in C. monnieri was detected by UHPLC-ESI-Q-TOF/MS. Quadrupole TOF/MS in either full scan mode or extracted ion mode was used for the qualitative analysis of the constituents. Relative peak area of each component was used for the hierarchical cluster analysis. Results According to UHPLC-ESI-QTOF-MS data, chemical structures of 28 coumarins in the fruits of C. monnieri were identified, including 19 simple coumarins, seven linear coumarins, and two angular coumarins. Among these constituents, ten coumarins were firstly identified in C. monnieri. In addition, hierarchical cluster analysis suggested that C. monnieri from different regions could be classified into four groups, and this clustering was correlated to the distribution significantly, Xuzhou could be regarded as the genuine producing area. Conclusion UHPLC-ESI-Q-TOF-MS is a viable method for qualitative analysis and quality evaluation of coumarins from the fruit of C. monnieri. Coumarins in C. monnieri exists intra-species variance, which indicates significant meaning for the quality control and choice of famous region drug for C. monnieri in the clinic medication.
