目的采用氢核磁脉冲宽度定量法(Pulse length based concentration determination,PULCON)对玄参对照提取物中的哈巴苷、安格洛苷C和哈巴俄苷进行定性及定值研究,探讨玄参对照提取物代替相应对照品在提升玄参复方制剂质量控制水平的可...目的采用氢核磁脉冲宽度定量法(Pulse length based concentration determination,PULCON)对玄参对照提取物中的哈巴苷、安格洛苷C和哈巴俄苷进行定性及定值研究,探讨玄参对照提取物代替相应对照品在提升玄参复方制剂质量控制水平的可行性。方法采用Bruker Avance III HD 700超导核磁共振波谱仪,以DMSO-d6为溶剂,苯甲酸为外标物,利用PULCON法比较苯甲酸定量峰(δ_(H)7.94)的峰面积和不同批次玄参对照提取物中3种化学成分的不同定量峰(哈巴苷δ_(H)6.24、安格洛苷Cδ_(H)7.08和哈巴俄苷δ_(H)5.97)的峰面积,测定不同批次中3种成分的含量,并采用配对t检验将测定结果与高效液相色谱法(High performance liquid chromatography,HPLC)的定值结果进行比对。分别以已知含量的玄参对照提取物和3个相应对照品为对照,建立增液汤的HPLC含量测定方法,采用配对t检验对2种方法所得结果进行比较。结果采用PULCON法测得3种成分的含量与HPLC法的定值结果基本一致,以玄参对照提取物为对照,3种成分的线性关系相关系数均大于0.9997,平均回收率为99.36%~102.31%。t检验结果显示,2种方法测定的哈巴苷、安格洛苷C、哈巴俄苷含量P值分别为0.279、0.105、0.623,均大于0.05,表明2种含量测定方法差异无统计学意义。结论PULCON法可在无对照品且无需分离的条件下,直接、快速、准确地分析玄参对照提取物成分的物质组成和含量,并将已标定准确含量的玄参对照提取物用于玄参复方制剂的质量控制,为中药对照提取物在中药质量研究中的应用提供了科学依据。展开更多
The orientation of melittin binding to liposomes with of without transmembrand potential was investigated.With The combination of high performance liquid chromatography and mass spectromeny, we detected The membrane a...The orientation of melittin binding to liposomes with of without transmembrand potential was investigated.With The combination of high performance liquid chromatography and mass spectromeny, we detected The membrane association state of melittin by analyzing its proteolytic products .We found that The enzyme could access ail The proteolyticc sites on protein binding to liposome without membrane potential.while one proteolytic site on The N-terminal of The Protein was blocked de it binding to liposome with negative transmembrane potential The results show that melittin reorients in The latter case.展开更多
Triethyl Phosphite is the intermediate of producing nervous toxin of organic phosphate,which is involved in the chemicals of schedule 3. in Convention On The Prohibition Of The Development,Production,Stockpiling And U...Triethyl Phosphite is the intermediate of producing nervous toxin of organic phosphate,which is involved in the chemicals of schedule 3. in Convention On The Prohibition Of The Development,Production,Stockpiling And Use Of Chemical Weapons And On Their Destruction.A method for the determination of triethyl phosphate was established by GC-MS/SIM.Average recovery was 96.3%-111.5% with linear range between concentration and peak area varying from 0.546-10.928 mg/L and the detection limits were 0.011 ng.展开更多
文摘目的采用氢核磁脉冲宽度定量法(Pulse length based concentration determination,PULCON)对玄参对照提取物中的哈巴苷、安格洛苷C和哈巴俄苷进行定性及定值研究,探讨玄参对照提取物代替相应对照品在提升玄参复方制剂质量控制水平的可行性。方法采用Bruker Avance III HD 700超导核磁共振波谱仪,以DMSO-d6为溶剂,苯甲酸为外标物,利用PULCON法比较苯甲酸定量峰(δ_(H)7.94)的峰面积和不同批次玄参对照提取物中3种化学成分的不同定量峰(哈巴苷δ_(H)6.24、安格洛苷Cδ_(H)7.08和哈巴俄苷δ_(H)5.97)的峰面积,测定不同批次中3种成分的含量,并采用配对t检验将测定结果与高效液相色谱法(High performance liquid chromatography,HPLC)的定值结果进行比对。分别以已知含量的玄参对照提取物和3个相应对照品为对照,建立增液汤的HPLC含量测定方法,采用配对t检验对2种方法所得结果进行比较。结果采用PULCON法测得3种成分的含量与HPLC法的定值结果基本一致,以玄参对照提取物为对照,3种成分的线性关系相关系数均大于0.9997,平均回收率为99.36%~102.31%。t检验结果显示,2种方法测定的哈巴苷、安格洛苷C、哈巴俄苷含量P值分别为0.279、0.105、0.623,均大于0.05,表明2种含量测定方法差异无统计学意义。结论PULCON法可在无对照品且无需分离的条件下,直接、快速、准确地分析玄参对照提取物成分的物质组成和含量,并将已标定准确含量的玄参对照提取物用于玄参复方制剂的质量控制,为中药对照提取物在中药质量研究中的应用提供了科学依据。
文摘The orientation of melittin binding to liposomes with of without transmembrand potential was investigated.With The combination of high performance liquid chromatography and mass spectromeny, we detected The membrane association state of melittin by analyzing its proteolytic products .We found that The enzyme could access ail The proteolyticc sites on protein binding to liposome without membrane potential.while one proteolytic site on The N-terminal of The Protein was blocked de it binding to liposome with negative transmembrane potential The results show that melittin reorients in The latter case.
文摘Triethyl Phosphite is the intermediate of producing nervous toxin of organic phosphate,which is involved in the chemicals of schedule 3. in Convention On The Prohibition Of The Development,Production,Stockpiling And Use Of Chemical Weapons And On Their Destruction.A method for the determination of triethyl phosphate was established by GC-MS/SIM.Average recovery was 96.3%-111.5% with linear range between concentration and peak area varying from 0.546-10.928 mg/L and the detection limits were 0.011 ng.
