HPLC-ELSD测定浙贝母中贝母素甲、贝母素乙的含量

 目的建立HPLC-ELSD测定浙贝母中贝母素甲、贝母素乙含量的方法,并对市售17批样品进行考察,制定含量限度。方法色谱柱:Agilent Hypersil BDS-C₁₈(4.0 mm×250 mm,5μm);流动相:乙腈-水-二乙胺(70:30:0.03),流速:0.8 mL·min^-1; ELSD参数:漂移管温度为85℃,载气流速为2.2 L·min^-1。结果贝母素甲、贝母素乙线性范围分别为47.02～1 003.46.92～1 001 mg·L^-1,平均回收率分别为102.7%,98.7%,RSD分别为2.1%,2.5%(n=6)。通过市售17批样品中贝母素甲、贝母素乙含量的测定,制定了不同规格浙贝母的含量限度。结论此法简便,快捷,结果可靠,可用于浙贝母的质量评价,为2005年版药典中浙贝母质量标准的修订提供了依据。     

不同溶媒对浙贝母生物碱含量影响的研究

目的：比较不同溶媒对浙贝母生物碱含量的影响。方法：采用比色法及薄层扫描法测定。结果：总生物碱、贝母素甲、贝母素乙的含量,水提最低,其次是95%乙醇、60%乙醇、甲醇、70%乙醇,结论：以甲醇及70%乙醇为溶媒提取浙贝母生物碱的含量最高。     

中药川贝母定量分析方法研究

目的:研究常用中药川贝母的定量分析方法。方法:应用高效液相色谱法。以4种川贝母共有的有效成分贝母辛为指标;采用AgilentHypersilBDS C₁₈(4. 0mm×2 5 0mm ,5 μm)色谱柱,以乙腈水 二乙胺(37∶6 3∶0 .0 3)为流动相,流速1 0mL·min^-1;Alltech 2 0 0 0蒸发光散射检测器检测,外标两点法定量。结果:贝母辛在0 . 0 3188～1. 0 2 0mg·mL^-1呈线性,回收率为10 2. 1% (n=5 ) ,RSD 3. 86 %。根据33批不同产地或来源的川贝母药材中贝母辛的含量结果,确定贝母辛的含量限度为0 . 0 0 70 %。结论:本法为良好的贝母辛的定量分析方法,可用于川贝母药材的质量控制。     

从百合病论治自主神经功能紊乱

百合病和自主神经功能紊乱的临床表现都以主观症状较突出、客观体征不显著、无明显器质性病变为特点,且发病范围广泛,可涉及多个脏腑。二者病因均与久病或精神情志异常有关。研究发现,治疗百合病常用的百合及百合类方与治疗自主神经功能紊乱的B族维生素、谷维素及抗抑郁、抗焦虑药物在功效上具有相似性。因此,临床可通过辨病、辨证将百合病的治疗经验应用到自主神经功能紊乱的治疗中,中西互补,以获良效。     

气相色谱-质谱联用法测定浙贝母中20种农药残留

目的:建立一种同时测定浙贝母中20种有机氯、拟除虫菊酯类农药残留量的分析方法。方法:样品用乙腈超声提取,经过Florisil固相萃取柱净化样品,用GC-MS选择离子模式进行测定,采用内标法进行定量,以3个添加水平测定样品的回收率和RSD。结果:回收率在67.7%～131.8%之间,RSD均低于15%。各农药检测限均小于0.01 mg.kg-1。结论:采用该方法测定浙贝母中20种有机氯及拟除虫菊酯类农药残留量,简单,快速,准确,灵敏,且重复性好,可用于浙贝母中多种农药残留的同时测定。     

Epidermoid cyst of the brain stem symptomatic in childhood

Background Epidermoid cysts may remain asymptomatic for a long period of time due to their slowly growing pattern corresponding with the normal human skin turnover time and due to soft and light cyst content. They do not cause compression of neural and vascular structures initially that is why almost all of the cases in the literature are diagnosed during adulthood.Methods We report here an epidermoid cyst in childhood, which was located in the medulla oblongata, unusually and atypically with liquefied cyst content. The liquefaction may occur due to an intrauterine or early childhood infection. The reported case also suffered previously a severe respiratory infection. Although the cyst is located in and around a highly eloquent neural area, plasticity of the brain stem prevented neurological deterioration due to this very slow growing extraaxial mass lesion. The ordinary cyst content found in the center of the cyst cavity during the operation suggested that the same ordinary material, which was previously at the periphery, ran to get liquefied in time.Conclusion We suggest that the symptoms of this present case appeared very early due to liquefaction of the cyst content with compression and displacement of the brain stem caudally. The recent infection process may predispose the pathological condition.     

Die zerebrovenöse fiberoptische Katheteroxymetrie im Hirndruckmodell des Schweins

The reliability of continuous fibreoptic oximetry in cerebral venous blood and its correlation with intracranial and cerebral perfusion pressures (pressure-volume curve) were examined in an experimental porcine study. Methods: The pressure in the infratentorial compartment of 13 domestic pigs (18–24?kg) was gradually increased by inflating a Fogarty balloon catheter placed on the surface of the right cerebellar hemisphere and below the tentorium. Single volumes of 0.4?ml saline were injected into the inflatable balloon at 1-min intervals up to a total volume of 7?ml. Intracranial pressure (ICP), arterial blood pressure, cerebral perfusion pressure (CPP), and cerebral venous saturation measured continuously by fibreoptic oximetry and intermittent blood-gas analyses (SjO₂ superior sagittal sinus) were monitored during balloon inflation. All data were downloaded onto a PC and evaluated off-line by a commercial statistical software package. Results: Over the whole pressure-volume curve, two phases of SjO₂ behaviour were registered by continuous fibreoptic oximetry (Oximetrix 3, Abbott) (Fig.?1). CPP ranges of less than 50% reduction from the initial value showed a linear correlation (r _mittl. =0.712, P<0,01) between both parameters (CPP?SjO₂). In CPP ranges below a crucial point of about 50?mmHg no such correlation was found (r _mittl =0.176, P>0.5). In contrast, in 3 pigs a very good correlation was found between CPP and SjO₂ over the whole pressure-volume curve as measured by blood-gas analyses of samples from the cerebrovenous catheter (r _mittl. =0.84, P<0.05). Discussion: We conclude that in physiological CPP ranges down to 50?mmHg, SjO₂ measurement is a reliable method of detecting oxygen desaturation in cerebrovenous blood. Below that CPP value, the fibreoptic catheter showed repeated false-high oxygen saturation values. The accuracy of SjO₂ measurement seems to depend on sufficient cerebral blood flow (CBF): with decreasing CBF the amount of cerebral venous outflow is diminished. We believe this is why we could not find a correlation in low CPP ranges with the oximetry catheter. This flow-dependency is a new aspect of fibreoptic cerebrovenous oximetry. The authors recommend that rising SjO₂ values after desaturation events be confirmed by blood-gas analyses.     

平贝母药材质量控制中适宜测定指标的研究

目的:通过对平贝母中平贝碱甲、贝母素甲、贝母素乙3个单体生物碱成分以及总生物碱测定结果的比较研究,确定可控制平贝母质量的合理测定指标。方法:采用 HPLC—MS 法,色谱柱为 Alltima C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.03%二乙胺(30∶70),流速:1 mL·min~(-1);质谱离子源为 ESI;检出模式为正离子检测;电离电压为3.2 kV;电喷雾接口干煤气(N_2)流速为300 L·h~(-1),离子源温度为105℃,锥孔电压为30 V;脱溶剂温度为150℃。选择离子质量数:464.7(平贝碱甲)、432.7(贝母素甲)、430.7(贝母素乙)。测定平贝母中平贝碱甲、贝母素甲、贝母素乙的含量。另以三氯甲烷-甲醇(4∶1)混合溶剂提取总生物碱,以溴麝香草酚蓝比色法在 pH 4.2,紫外吸收波长413 nm 下测定平贝母中总生物碱的含量,结果:LC—MS 法测定平贝母中平贝碱甲、贝母素甲、贝母素乙的含量分别为5～19,1～3,2～3μg·g~(-1);溴麝香草酚蓝比色法测定总生物碱含量以贝母素乙计为600～1000 μg·g~(-1)。结论:平贝母中单-生物碱成分含量太低,不宜作为平贝母药材的质量控制指标,以溴麝香草酚蓝比色法测定总生物碱含量可更客观反映平贝母药用物质情况,更适用于平贝母药材的质量控制。     

清肺通络膏的体外经皮渗透试验考察

目的:研究清肺通络膏中大黄游离蒽醌类成分的体外透皮吸收特性,考察辅药大蒜对各成分透皮特性的影响。方法:以清肺通络膏中主要成分芦荟大黄素、大黄素、大黄酸为指标,采用体外透皮吸收试验及HPLC考察该制剂的体外透皮特性,并评价该制剂不同配伍组中指标性成分的累积透过量及渗透速率。结果:大黄素的单位面积累积透皮量及透皮速率最大,芦荟大黄素次之,大黄酸最小;大黄酸的透皮时滞最长(0.419 h),大黄素时滞最短(0.006 h);清肺通络膏中大黄素、大黄酸、芦荟大黄素的体外经皮渗透曲线分别为Q=12.144t-14.880(r=0.97),Q=10.111t-3.886(r=0.93),Q=1.389t-0.583(r=0.95)。全方组中大黄素、芦荟大黄素、大黄酸的8 h累积透过量为分别为(86.059±0.168),(83.079±3.303),(12.819±0.569)μg·cm~(-2),透皮速率分别为12.144,10.111,1.389μg·cm~(-2)·h~(-1),与主药组比较有显著性差异(P0.05)。结论:清肺通络膏的体外经皮渗透符合零级动力学过程,大蒜对清肺通络膏中指标性成分的经皮渗透有促进作用。     

新疆伊贝母有效成分含量与土壤因子相关性分析

目的:研究伊贝母有效成分含量与土壤因子的相关性,筛选影响其有效成分含量的主导因子。方法:理化分析法进行土壤因子(pH,总盐,有机质,全氮,全磷,全钾,速效氮,速效磷,速效钾)的测定,应用主成分分析、聚类分析、相关分析及灰色关联度分析进行综合分析。结果:新疆不同产地土壤因子的含量存在较大差异,在同一产地的土壤因子含量也存在一定差异。总生物碱含量与速效钾有极显著正相关(P0.01),与总盐有显著正相关(P0.05);西贝母碱与9种土壤因子无明显的相关性;西贝母碱苷含量与总盐有显著正相关(P0.05);水溶性成分腺苷含量与总盐、有机质、全氮、速效氮、速效钾有极显著正相关(P0.01),β-胸苷含量与全氮有显著正相关(P0.05)。上述相关分析结果与灰色关联度分析结果一致。伊贝母最佳适宜生长的土壤条件为pH 6.4~6.9,总盐2.3~5.6 g·kg~(-1),有机质118~231 g·kg~(-1),全氮5.8~11.9 g·kg~(-1),全磷0.85~1.28 g·kg~(-1),全钾10.4~29 g·kg~(-1),速效氮428~906 mg·kg~(-1),速效磷31~57 mg·kg~(-1),速效钾424~494 mg·kg~(-1)。结论:综合考虑,土壤中速效钾、全氮、有机质、速效氮及总盐对伊贝母中有效成分的合成和积累起到了关键性作用。因此,无论选择土壤,还是生产中施肥,都应重视和合理使用速效钾、全氮、有机质、速效氮及总盐对伊贝母质量的影响。