【作者】 孙晓梅；

【导师】 杨祥良； 代东梅；

【作者基本信息】 华中科技大学 ， 有机化学， 2007， 硕士

【摘要】 本研究对麝香壮骨膏的化学成分、各组分的药理学研究和现有状况进行了综述,建立了同步测定麝香壮骨膏中樟脑、薄荷脑、冰片和水杨酸甲酯等四种成分含量的气相色谱方法。挥发油测定器蒸馏制备供试液,萘为内标物,PEG-20M为固定相的毛细管柱,氮气为载气,检测器为FID,采用程序升温,用内标法测定样品中四种成分的含量。麝香壮骨膏中的樟脑、薄荷脑、冰片(龙脑和异龙脑)和水杨酸甲酯及内标物萘等五种物质在同一色谱条件下获得良好分离,樟脑、薄荷脑、冰片和水杨酸甲酯的回收率依次为96.92%(RSD=2.42%),98.03%(RSD=1.81%),99.02%(RSD=1.47%)和98.15%(RSD=1.59%)。采用此方法对麝香壮骨膏的六个不同厂家的产品进行含量测定,均可取得较好的结果。该方法简便、准确、分离度好,可用于控制此类组分的质量。研究了用挥发油提取器提取四种组分时提取条件对其提取率的影响,通过单因素试验确定提取次数、提取时间、加水量的大致范围,并在单因素考察的基础上设计正交试验表,试验结果表明:提取次数为1次、提取时间为4 h、加水量为150 mL时的提取率最好。建立高效液相色谱法限量测定麝香壮骨膏中乌头碱的含量,三种方法处理样品,外标法定量,Hypersil ODS2 C18色谱柱,紫外检测器,检测波长为233 nm,流动相为甲醇-0.05%三乙胺(70:30)。乌头碱在此条件下峰形较好,线性范围为0.08~1.60μg, r=0.9988,最低检测限为3 ng,精密度为1.29% (n=6),乌头碱的回收率为98.65%(RSD= 0.62%)。采用此方法对麝香壮骨膏中的乌头碱进行测定,取得了较好的结果,该方法可作为乌头碱质量控制方法。更多还原

【Abstract】 The phytochemical and pharmacological researches of some component on Shexiang Zhuanggu Plaster were summarized in the thesis. The method for the simultaneous determination of camphor, menthol, synthetic borneol and methyl salicylate in Shexiang Zhuanggu Plaster was established by gas chromatography. The sample solution was prepared by distillation with essential oil collector. Naphthalene is the internal standard. The GC system consisted of capillary column, PEG-20M as the stationary phase, nitrogen as the carrier gas, FID as the detector. The programmed temperature-GC and internal standard method was employed to determine four kinds of components in Shexiang Zhuanggu Plaster. Camphor, menthol, synthetic borneol (borneol and isoborneol) and methyl salicylate in Shexiang Zhuanggu Plaster and naphthalene have been separated well under the same chromatographic condition. The average recovery of camphor, menthol, synthetic borneol and methyl salicylate were 96.92%(RSD=2.42%), 98.03%(RSD=1.81%), 99.02%(RSD= 1.47%) and 98.15%(RSD=1.59%),respectively. The method is simple, accurate and separable, and can be used to control the quality of the four kinds of components.The article studied the effects of extraction condition on the percentage of the extraction of four components with essential oil collector. The probable range of the number of extraction, extraction time and water amount were obtained through one factor experiments, and the orthogonal experiments were designed based on one factor experiments. The results showed that the extraction obtained under the condition of number 1, time 4 h, water amount 150 mL has the highest percentage of the extraction.For the purpose of the limited determination of aconitine in Shexiang Zhuanggu Plaster, High Performance Liquid Chromatography method was established. The sample solution was prepared by three kinds of methods. External reference method was employed to determine aconitine in Shexiang Zhuanggu Plaster. The HPLC system consisted of Hypersil ODS2 C18 column, VWD as the detector. Detected Wavelength is 233 nm, Methanol-0.05% triethylamine(70:30) as flowing phase. The linear range was 0.08~1.60μg, r=0.9988. The detective limit was 3 ng, The precision for aconitine was less than 1.29% (n=6), The recoveries of aconitine was 98.65% (RSD=0.62%) in shexiang zhuanggu plaster respectively. The method can be used as a limited quantitative analysis of aconitine .更多还原