【作者】 王仲；

【导师】 张长弓；

【作者基本信息】 华中科技大学 ， 生药学， 2008， 硕士

【摘要】 搏心通的原药材葱白为百合科植物分葱Allium fisturosum L. var. caespitosum Makio的干燥鳞茎,性辛温,功效发表、通阳、解毒,可治疗多种疾病。采用超临界CO2萃取技术(SFE )提取搏心通原料药,并对原料药运用气质联用技术进行化学成分分析,检索出了八类成分:有机硫化物、有机胺、杂环化合物、醛、酮、酯、脂肪酸(酯)、长链烷烃。我们还与传统的水蒸气蒸馏法(SDE)进行了比较研究。通过查阅文献资料和药理实验,证明其中的有机硫化物和脂肪酸两类成分为搏心通的有效成分,并针对这两类成分的结构进行详细的分析。本实验将脂肪酸衍生化成相应的酯(甲基酯)解决了脂肪酸GC中拖尾的问题,然后进行GC-MS检索,分离并鉴定出9种脂肪酸(甲酯),计算出它们的相对百分含量。含量较高的依次是亚油酸甲酯(C19H34O2) 62.44%、棕榈酸甲酯(C17H34O2) 21.34%、亚麻酸甲酯(C19H3202) 9.65%。在对有机硫化物的分析中,本实验从生源途径入手,针对硫化物形成过程,来验证检索结构的准确程度。由于搏心通软胶囊原料药为油脂类成分,本实验按照药典(附录IX N)上规定对其理化常数进行了测定,从而确定酸值、皂化值、羟值、碘值的有效范围应分别控制在为40~43、177~180、127~130、40~43。实验采用气相色谱法对脂肪酸类成分的质量进行研究。首先确立最佳的色谱条件,色谱柱为:HP-INNOWAX(30 m×0.53 mm×1 um),程序升温法:120℃保持2 min,以10℃/min的速度升到180℃,保持2 min,以2℃/min速度升到184℃,以1℃/min速度升到190℃;然后采用甲酯化法对样品进行衍生化处理,方法学考察结果表明精密度良好,加样回收率为97%~103%。证明该方法操作简便,结果准确可靠。运用元素分析仪测定药物总硫,方法学考察结果表明:精密度良好,加样回收率为99%~104%,证明了该方法准确可行。结合化学成分分析的结果,将硫元素全部换算成含量最高的2,5-二甲基噻吩的含量,为8.6%。更多还原

【Abstract】 The original medicines of boxintong come from Allium fisturosum L. var. caespitosum Makio which is a plant belonging to family of lily, genera of shallot. It has been used as folk medicine to treat many diseases.The chemical compositions of raw materials of boxintong (SFE) have been studied by GC-MS method. Eight kinds of constituents were got and identified, which are organic sulfide compounds, organic amine, heterocycles, aldehyde, ketone, ester, fatty acid (ester), and long-chain alkanes, compairing with traditional method steam distillation extraction(SDE). Organic sulfide compounds and fatty acid have a lot of effect on pharmacological aspects and extensive curative effects by researchs and reports.Nine fatty acid compounds were also got and identified by GC-MS. The total content of the fatty acids was 7%. The content of linoleic acid was the highest (62.44%)and palmitic acid was the next (21.34%). In the research of organic sulfide compounds, we analysis their structures by biogenesis pathway.As fatty oil, we determine physicochemical constant of boxintong with method from the Chinese Pharmacopoeia. So that we could provisions the effective ranges of the raw materials: acid value 40~43, saponification value 177~180,hydroxyl value 127~130, iodine value 40~43.A capillary gas chromatographic (GC) method equipped with flame ionization detection was developed for the simultaneous analysis of linoleic acid in boxintong. Compounds were separated on an HP-INNOWAX(30 m×0.53 mm×1 um). The polar column was 120℃for 2min programmed to 180℃at 10℃/min, 180℃for 2 min, programmed to 184℃at 2℃/min, 184℃for 1 min, programmed to 190℃at 1℃/min.;detector temperature 250℃. The orthogonal design was adopted to optimize the derivation reaction conditions of fatty oil. The calibration curves were linear in the range of 0.107~0.321 ug (R2=0.9991) . The average recovery of linoleic acid was 97% ~103% (RSD=1.3%). The assay method was simple, rapid, reliable and reproducible and provided a quantitative basis for the quality assessment of boxintong.Determine the total sulfide element of drugs by elemental Analyzers at the first time. The result shows that its precision was under 3%, and the recoveries ranges were of 99%~104%. The proposed method is rapid and suitable for the determination of total sulfide element. Then all sulfide elements will be converted to organic sulfide 2,5 - dimethyl thiophene the highest content. It is 8.6%.更多还原