止咳平喘颗粒的质量标准研究简

为建立止咳平喘颗粒的质量标准,本试验采用薄层色谱法（TLC）对组方中紫菀、桑白皮、百部、枇杷叶及鱼腥草进行定性鉴别,采用高效液相色谱法测定本方中紫菀酮的含量。结果显示,TLC鉴别专属性强,斑点清晰;采用C₁₈反相柱,以乙腈—水为流动相,检测波长为200 nm,其线性范围为10.2～510.0 μg/mL,回归方程为A＝11481C＋36617（R²＝1,n=6）。平均回收率为99.89%,RSD=1.57%。本试验所建立的方法简便、准确、专属性强、重复性好,可有效地控制颗粒的质量。     

防己散质量控制方法研究

对<中国兽药典>2005年版防己散的质量标准进行修订,采用薄层色谱法对制剂中防己药材进行定性鉴别,采用高效液相色谱法对粉防己碱和防己诺林碱进行了含量测定.建立了同时测定防己散中2种成分含量的方法,粉防己碱和防己诺林碱的线性范围分别为52.55～525.5μg/ml(r=0.999 5)和27.30～273.0 μg/ml(r=0.999 6):平均回收率(n=9)分别为98.1%(RSD=1.9%)和97.9%(RSD=2.2%).该方法简便、准确、重复性好,为防己散的质量控制提供了定量方法.     

两种薄层色谱法鉴别双黄连口服液中黄芩苷、绿原酸的探讨

双黄连口服液标准分别收载于《中国兽药典》2000年版[1]和2005年版[2]二部中,改版收载于2005年版二部,对【鉴别】项(1)方法进行了修订,其他检测项目相同。现按照2005年版二部收载双黄连口服液检测产品时,对【鉴别】项(1)方法有些见解,提出与大家探讨,通过反复试验,实验结果表明,按本方法在紫外光灯(254nm)下检视结果时,供试品色谱中无斑点,与对照品色谱相应位置上,未见斑点,致使无法判定结果,见图2。在紫外光灯(365nm)下检视,供试品色谱中,在与对照品色谱相应位置上,显相同颜色的荧光斑点,但Rf值小,分离度不高(见图4)。     

心悦滴丸的质量标准研究

目的建立心悦滴丸的质量标准。方法采用TLC对心悦滴丸中西洋参茎叶总皂苷进行定性鉴别;采用HPLC测定人参皂苷Rb2、Rb3、Rd的含量,色谱条件为Agilent ODS C18色谱柱(4.6mm×250mm,5 m),乙腈-0.05%磷酸水溶液为流动相梯度洗脱,流速1.0m L/min,检测波长203nm,柱温40℃。结果心悦滴丸中西洋参茎叶总皂苷的薄层色谱斑点清晰。人参皂苷Rb2在0.748~4.704μg范围内呈良好线性关系(r=0.9999),平均回收率为96.2%(RSD1.9%);人参皂苷Rb3在1.632~9.792μg范围内呈良好线性关系(r=0.9999),平均回率为97.5%(RSD1.7%);人参皂苷Rd在0.96~5.76μg范围内呈良好线性关系(r=0.9999),平均回收率为96.6%(RSD2.1%)。结论建立的方法操作简便、专属性强、灵敏度高、重复性好,可作为心悦滴丸的质量控制标准。     

白黄散胶囊质量标准的研究

建立了白黄散胶囊的质量标准。用薄层色谱法鉴别白头翁、黄芪、黄连、黄柏、山楂、乌梅、诃子,以高效液相色谱法测定盐酸小檗碱的含量。结果薄层色谱图斑点清晰,阴性对照无干扰,盐酸小檗碱在9.91～148.65μg/mL范围内与峰面积线性关系良好,加样回收率为97.70%,RSD为1.30%。所建立的方法简便、准确、重现性好,可用于白黄散胶囊的质量控制。     

云南大白口蘑子实体中秋水仙碱含量的TLC法测定研究

采用超声法提取云南大白口蘑子实体中的秋水仙碱,并用薄层扫描法来测定其含量。结果表明:λ=352 nm,秋水仙碱线性范围为0.08～0.94μg,相关系数为0.9994,平均回收率为99.65%,RSD=3.98%;该法准确、简便、快速、重复性好,适用于优质单株的高通量筛选。     

肥猪散中制何首乌的薄层鉴别方法研究

建立了肥猪散中制何首乌的薄层色谱(TLC)定性鉴别法。以制何首乌为对照药材,采用甲苯-乙酸乙酯-甲酸(15:2:0.8)为展开剂,在UV365nm波长下检视,氨蒸气为显色剂,对肥猪散中制何首乌进行薄层色谱法鉴别。结果制何首乌斑点清晰,阴性无干扰。本方法简便,快速,结果准确,重现性好。可用于控制肥猪散的质量。     

Separation of liquefied product of Salix psammophila by column chromatography and structure analysis of its components

The liquefied product of Salix psammophila wood was separated by thin-layer chromatography (TLC) and column chro-matography, and its structure was identified by nuclear magnetic resonance (NMR) spectra in our study. The separation result indi-cates that the sample of liquefied S. psammophila contained at least two categories of components. The structure of the main compo-nents was guaiacyl C-1, C-2 of the hydroxyphenyl propane, i.e., the aromatic nucleus protons of lignin. Degradation and polycon-densation reactions occurred when the S. psammophila wood was liquefied in phenol. Polycondensation reactions occurred among the depolymerization products from cellulose, the aromatic depolymerization products from lignin and the products of the displace-ment reactions between phenoxide ion and cellulose.     

New cholinesterase inhibiting bisbenzylisoquinoline alkaloids from Abuta grandifolia

The phytochemical study of the stem bark and wood of Abuta grandifolia (Mart.) Sandwith led to the identification of four bisbenzylisoquinoline alkaloids (BBIQs), namely (R,S)-2 N-norberbamunine (1), (R,R)-isochondodendrine (2), (S-S)-O4″-methyl, Nb-nor-O6'-demethyl-(+)-curine (3), and (S-S)-O4″-methyl, O6'-demethyl-(+)-curine (4), together with the aporphine alkaloid R-nornuciferine (5), all obtained by countercurrent distribution separation (CCD) and identified on the basis of their spectroscopic data. Alkaloids 3 and 4 were new. All the isolated compounds were tested for acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) inhibitory activities. 1 was the most active against AChE, whereas 3 and 4 were the most potent against BChE. Interestingly, all tested alkaloids are more potent against BChE than against AChE. This selectivity of cholinesterase (ChE) inhibition could be important in order to speculate on their potential therapeutic relevance.     

蜂蜜中掺入不同类型果葡糖浆的检测

采用薄层色谱法检测蜂蜜中掺有的不同类型的果葡糖浆。果葡糖浆中的高分子糖经活性炭-硅藻土柱的富集、浓缩,再用(1+1)乙醇溶液洗脱,最后用薄层色谱法分离、检测。实验证明,薄层色谱法可检测出蜂蜜中掺入的F42和F55类型的果葡糖浆,而无法鉴别掺入的F90类型的果葡糖浆。