中药青风藤、川芎中生物碱的分析研究
摘要
本文利用GC-MS和FAB-MS对中药青风藤和川芎中的生物碱进行了研究。
全文共分为四章：
第1章主要阐述了生物碱的类型、理化性质、测定方法,以及GC-MS和FAB-MS在生物碱分析中的应用。
第2章采用气相色谱-质谱联用方法,分析中草药青风藤中的生物碱。共分离鉴定出生物碱,稠环类和酚类物质等22种化合物。其中青藤碱含量较高,并具有一种同分异构体,它的质量分数比青藤碱约高2.69%,其它种生物碱含量较低。
第3章利用自制的树脂与盐酸川芎嗪制备分子印迹吸附树脂,该树脂对盐酸川芎嗪的吸附率达到85%；用这种具有川芎嗪识别点的树脂,制成固相萃取柱分析川芎中的川芎嗪,川芎嗪的提取率比常规处理样品的提取率提高了近30倍。实验中还根据溶剂的极性分别用水、丙酮和三氯甲烷等三种溶剂对固相萃取柱的洗脱效果进行了研究,发现丙酮在三者中具有最好的洗脱效果。
第4章利用在FAB-MS分析中,离子峰强度随时间衰减的关系,建立了一种用FAB-MS定量分析川芎嗪的方法。在FAB-MS分析中,被测样品的分子离子峰强度呈指数衰减。对其作非线性拟合,发现其初始峰强的比值与样品浓度呈线性,选择合适的内标物,就可对样品定量分析。实验中以激光照射0.5h下,川芎嗪的氘代产物为内标物,得到川芎嗪定量分析的工作曲线的线性方程为y=6.75+2.24 x(R=0.99084),精密度RSD=2.86%。并用此方法对药品磷酸川芎嗪片剂进行了分析。
The alkaloids from Sinomenium acutum Rehd. et Wils and Ligusticum Chuanxiong Hort. are analyzed by GC-MS and FAB-MS.
The total paper consists of four chapters.
Chapter one:The types, physicochemical property, and measuring method of alkaloids are reviewed, and the applications of GC-MS and FAB-MS in alkaloids are also reviewed.
Chapter two:Alkaloids from Sinomenium acutum stem are analyzed by GC-MS. From the mass spectrometry,22 kinds of compounds are identified, which are morphinan, indole, acridone, pyrone, and condensed ring and phenols compounds. By using peak area for comparison, it is found that the content of sinomenine is higher than other kinds of alkaloids. One isomeride of sinomenine is found with its mass fraction 2.69% higher than smomemne.
Chapter three:A new kind of molecularly imprinted adsorptive resin is prepared using ligustrazine hydrochloride as the template molecule. The adsorptive resin with ligustrazine recognition sites has an adsorbability of 85%. In the paper, ligustrazine is effectively separated and enriched from herbs by using a solid-phase extraction column filled with the imprinted adsorptive resin. Its eluent is analyzed by GC-MS, and the results indicate that the extraction rate of this imprinted adsorptive resin is nearly 30 times higher than current preparation. Three eluted solvents of different polar, which are water, acetone and chloroform, are also studied. It is found that acetone has the best eluted result.
Chapter four:It is found that the total ion's intensity of quasi-ion molecule takes on exponential decrease with time in fast atom bombardment mass spectrometry (FAB-MS), so a new method is based upon it for the quantitative analysis of ligustrazine. Fitting it by non-liner curve can calculate the initiatory total ion's intensity. The quasi-ion molecule peak initiatory total intensity ratio of the sample and internal standard is proportion to the concentration of tested sample; it can be applied to quantitative analysis for samples. In this paper deuteride ligustrazine which is radiated under laser for 0.5h, is used as internal standard. And the standard equation preparation, which is y= 6.75+2.24 x (R= 0.99084) is gotten. In this paper troche medicine of ligustrazine phosphate has been quantitative analysis.
全文共分为四章：
第1章主要阐述了生物碱的类型、理化性质、测定方法,以及GC-MS和FAB-MS在生物碱分析中的应用。
第2章采用气相色谱-质谱联用方法,分析中草药青风藤中的生物碱。共分离鉴定出生物碱,稠环类和酚类物质等22种化合物。其中青藤碱含量较高,并具有一种同分异构体,它的质量分数比青藤碱约高2.69%,其它种生物碱含量较低。
第3章利用自制的树脂与盐酸川芎嗪制备分子印迹吸附树脂,该树脂对盐酸川芎嗪的吸附率达到85%；用这种具有川芎嗪识别点的树脂,制成固相萃取柱分析川芎中的川芎嗪,川芎嗪的提取率比常规处理样品的提取率提高了近30倍。实验中还根据溶剂的极性分别用水、丙酮和三氯甲烷等三种溶剂对固相萃取柱的洗脱效果进行了研究,发现丙酮在三者中具有最好的洗脱效果。
第4章利用在FAB-MS分析中,离子峰强度随时间衰减的关系,建立了一种用FAB-MS定量分析川芎嗪的方法。在FAB-MS分析中,被测样品的分子离子峰强度呈指数衰减。对其作非线性拟合,发现其初始峰强的比值与样品浓度呈线性,选择合适的内标物,就可对样品定量分析。实验中以激光照射0.5h下,川芎嗪的氘代产物为内标物,得到川芎嗪定量分析的工作曲线的线性方程为y=6.75+2.24 x(R=0.99084),精密度RSD=2.86%。并用此方法对药品磷酸川芎嗪片剂进行了分析。
The alkaloids from Sinomenium acutum Rehd. et Wils and Ligusticum Chuanxiong Hort. are analyzed by GC-MS and FAB-MS.
The total paper consists of four chapters.
Chapter one:The types, physicochemical property, and measuring method of alkaloids are reviewed, and the applications of GC-MS and FAB-MS in alkaloids are also reviewed.
Chapter two:Alkaloids from Sinomenium acutum stem are analyzed by GC-MS. From the mass spectrometry,22 kinds of compounds are identified, which are morphinan, indole, acridone, pyrone, and condensed ring and phenols compounds. By using peak area for comparison, it is found that the content of sinomenine is higher than other kinds of alkaloids. One isomeride of sinomenine is found with its mass fraction 2.69% higher than smomemne.
Chapter three:A new kind of molecularly imprinted adsorptive resin is prepared using ligustrazine hydrochloride as the template molecule. The adsorptive resin with ligustrazine recognition sites has an adsorbability of 85%. In the paper, ligustrazine is effectively separated and enriched from herbs by using a solid-phase extraction column filled with the imprinted adsorptive resin. Its eluent is analyzed by GC-MS, and the results indicate that the extraction rate of this imprinted adsorptive resin is nearly 30 times higher than current preparation. Three eluted solvents of different polar, which are water, acetone and chloroform, are also studied. It is found that acetone has the best eluted result.
Chapter four:It is found that the total ion's intensity of quasi-ion molecule takes on exponential decrease with time in fast atom bombardment mass spectrometry (FAB-MS), so a new method is based upon it for the quantitative analysis of ligustrazine. Fitting it by non-liner curve can calculate the initiatory total ion's intensity. The quasi-ion molecule peak initiatory total intensity ratio of the sample and internal standard is proportion to the concentration of tested sample; it can be applied to quantitative analysis for samples. In this paper deuteride ligustrazine which is radiated under laser for 0.5h, is used as internal standard. And the standard equation preparation, which is y= 6.75+2.24 x (R= 0.99084) is gotten. In this paper troche medicine of ligustrazine phosphate has been quantitative analysis.
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