一清片多成分、多指标质量控制研究

目的:完善一清片的质量控制方法。方法:采用薄层色谱法对处方黄芩、大黄进行定性鉴别;采用高效液相色谱法测定黄芩苷、大黄素、大黄酚的含量;建立一清片中表小檗碱、黄连碱、巴马汀和小檗碱的一测多评方法;同时采用外标法测定上述4种生物碱的含量,比较计算值与实测值之间的差别。结果:薄层色谱中可检出黄芩、大黄,专属性强,阴性无干扰;本方法大黄素、大黄酚线性范围分别为5.21~156.24,10.96~328.80 ng;平均回收率分别为94.49%,93.88%;RSD分别为1.2%,1.6%(n=6);可用一测多评法测定一清片中4种原小檗碱型生物碱的含量,2种测定方法差异无显著。结论:本试验的方法可靠,结果准确,可运用于一清片的质量控制。     

Effects and uptake of gold nanoparticles deposited at the air-liquid interface of a human epithelial airway model

The impact of nanoparticles (NPs) in medicine and biology has increased rapidly in recent years. Gold NPs have advantageous properties such as chemical stability, high electron density and affinity to biomolecules, making them very promising candidates as drug carriers and diagnostic tools. However, diverse studies on the toxicity of gold NPs have reported contradictory results. To address this issue, a triple cell co-culture model simulating the alveolar lung epithelium was used and exposed at the air-liquid interface.The cell cultures were exposed to characterized aerosols with 15 nm gold particles (61 ng Au/cm² and 561 ng Au/cm² deposition) and incubated for 4 h and 24 h. Experiments were repeated six times. The mRNA induction of pro-inflammatory (TNFα, IL-8, iNOS) and oxidative stress markers (HO-1, SOD2) was measured, as well as protein induction of pro- and anti-inflammatory cytokines (IL-1, IL-2, IL-4, IL-6, IL-8, IL-10, GM-CSF, TNFα, INFγ). A pre-stimulation with lipopolysaccharide (LPS) was performed to further study the effects of particles under inflammatory conditions. Particle deposition and particle uptake by cells were analyzed by transmission electron microscopy and design-based stereology.A homogeneous deposition was revealed, and particles were found to enter all cell types. No mRNA induction due to particles was observed for all markers. The cell culture system was sensitive to LPS but gold particles did not cause any synergistic or suppressive effects.With this experimental setup, reflecting the physiological conditions more precisely, no adverse effects from gold NPs were observed. However, chronic studies under in vivo conditions are needed to entirely exclude adverse effects.     

一测多评法在舒肝健脾丸质量控制中的应用

目的：建立舒肝健脾丸一测多评的测定方法,验证此方法在舒肝健脾丸质量评价中应用的准确性、适应性和可行性。方法：将舒肝健脾丸为研究对象,以橙皮苷为内参物,建立橙皮苷与柚皮苷、柑属苷B的相对校正因子,并将校正因子应用于橙皮苷、柚皮苷和柑属苷B的含量测定,实现一测多评;同时采用外标法测定上述3种黄酮类成分的含量,比较计算值与实测值的差异。结果：线性考察Y橙皮苷=56 644X-2 272.9（r=0.999 8）;Y柚皮苷=41 070X+779.59（r=0.999 9）;Y柑属苷B=33 619X+2 289.8（r=0.999 9）,线性关系良好;校正因子,柚皮苷RSD 0.286%,柑属苷B RSD 0.259%;阴性无干扰,专属性良好;精密度,橙皮苷RSD 0.48%,柚皮苷 RSD 1.02%,柑属苷B RSD 0.97%;重复性,橙皮苷 RSD 0.94%,柚皮苷 RSD 0.89%,柑属苷B RSD 1.27%;回收率,橙皮苷平均回收率99.26%,RSD 0.90%,柚皮苷平均回收率99.30%,RSD 0.92%,柑属苷B平均回收率 98.34%RSD 0.78%,该方法准确、可靠;一测多评法柚皮苷含量为6.11,6.09,6.13 mg·g^-1,柑属苷B为 4.96,4.93,4.99 mg·g^-1,外标法柚皮苷含量为6.12,6.08,6.17 mg·g^-1,柑属苷B为 4.98,4.95,5.01 mg·g^-1,两种方法含量测定结果差异不显著。结论：一测多评法可同时对疏肝健脾丸中的橙皮苷、柚皮苷和柑属苷B进行含量测定,该方法简便、准确、可靠,可有效提高疏肝健脾丸的质量水平。     

一测多评法测定丹参中丹参酮ⅡA、隐丹参酮、丹参酮Ⅰ、二氢丹参酮Ⅰ的含量

目的:建立一测多评法同时测定丹参中丹参酮ⅡA、丹参酮I、二氢丹参酮I、隐丹参酮的含量,验证该方法在丹参药材中应用的准确性和可行性。方法:以丹参药材为研究对象,药材中4个有效成分为指标性成分,分别建立丹参酮ⅡA与二氢丹参酮I、隐丹参酮、丹参酮I的相对校正因子,计算二氢丹参酮I、隐丹参酮、丹参酮I的含量,实现一测多评。同时采用外标法测定药材中4个指标性成分的含量,比较计算值与实测值的差异,以验证一测多评法的准确性和可行性。结果:16批丹参中4个指标性成分,采用校正因子计算的含量值与外标法实测值之间无显著差异。结论:在对照品缺乏的情况下,以外标法测定丹参酮ⅡA,利用相对校正因子实现对二氢丹参酮I、隐丹参酮、丹参酮I的含量测定是可行的,一测多评法可以用于丹参中多种成分的质量评价研究。     

适合中药特点的质量评价模式——QAMS研究概述

在分析总结文献的基础上,概述了适合中药特点的质量评价模式———一测多评法(QAMS)的由来及其在中药质量评价中应用的可行性研究近况,针对该评价模式建立过程中涉及的关键问题进行了深入探讨,展望了QAMS在中药质量控制和评价中的应用前景。     

一测多评法测定藏药当佐中没食子酸、羟基红花黄色素-A、桂皮醛及胡椒碱的含量

目的:建立藏药当佐一测多评法,考察不同类型化合物之间采用相对校正因子进行含量测定的准确性和可行性。方法:以藏药当佐为研究对象,通过建立胡椒碱与其他3个指标成分间的相对校正因子(RCF),并利用校正因子对没食子酸、羟基红花黄色素-A、桂皮醛的含量进行计算,实现一测多评(计算法);同时采用外标法测定当佐中该4个指标成分含量(实测法),并比较计算值与实测值之间的差异。结果:在一定的线性范围内,胡椒碱与没食子酸、羟基红花黄色素-A、桂皮醛间的RCF分别为1.3686,0.2620,3.1333;且在不同实验条件下重现性良好(RSD分别为3.7%,2.2%,2.1%);不同来源当佐中4个成分含量的计算值与实测值间无明显差异(RSD<5%)。结论:本研究建立的只用1个对照品同步测定当佐中4个成分的一测多评法是准确的、可行的,可用于不同类型化合物间的含量测定,为民族药物多指标质量评价提供新的思路。     

Alkaline earth silicate wools – A new generation of high temperature insulation

Intensive study of the natural asbestiform minerals that cause human diseases, and the consequent understanding of their hazardous characteristics, has enabled the development of manufactured fibres whose physical and/or chemical properties, in particular as they relate to biopersistence, have been adjusted to minimize possible harm to health. A strong driver for the development of new high temperature insulation materials was the perception of the toxicity of refractory ceramic fibres (RCF) and their classification in the EU as a category 2 carcinogen under Directive 67/548/EEC. Such classification carries with it the requirement for substitution by less hazardous materials. This paper focuses on the development of alkaline earth silicate (AES) wools as a new class of high temperature insulation with the capability of such substitution in a number of applications. These wools have only a low potential to cause harm because they do not persist in lung tissue once deposited, and have produced minimal effects in experimental test systems. AES wools are increasingly being used in a wide range of high temperature applications.     

一测多评法同时测定肉桂药材中4种成分的含量

目的建立一测多评法同时测定肉桂药材中肉桂酸、香豆素、桂皮醛和邻甲氧基肉桂醛4种成分的含量,探究其在肉桂药材质量评价中的可行性。方法采用高效液相色谱法,以肉桂酸为内参,建立香豆素、桂皮醛和邻甲氧基肉桂醛与肉桂酸之间的相对校正因子,同时采用外标法和一测多评法测定其他3种成分的含量并进行比较,验证一测多评法在肉桂药材评价的准确性和可行性。结果该方法在不同实验条件下耐用性良好(RSD<3.0%);香豆素、桂皮醛和邻甲氧基肉桂醛3种化学成分相对于肉桂酸的相对校正因子分别为2.52、2.16、2.32;一测多评法和外标法分析结果差异无统计学意义。结论所建立的一测多评法准确度高、适用性强,可用于肉桂药材及其相关复方产品的质量评价。     

HPLC-QAMS同时测定屏风生脉胶囊中9个指标成分含量

目的 建立高效液相色谱一测多评法（HPLC-QAMS）同时测定屏风生脉胶囊中毛蕊异黄酮葡萄糖苷、芒柄花苷、9,10-二甲氧基紫檀烷-3-O-β-D-葡萄糖苷、芒柄花素、升麻素苷、升麻素、亥茅酚苷、麦冬甲基黄烷酮A及甲基麦冬二氢高异黄酮B含量的方法。方法 采用Agilent ZORAX StableBond C₁₈色谱柱（250 mm×4.6 mm,5 μm）,流动相乙腈-0.1%甲酸溶液,梯度洗脱。多波长切换检测（0~36 min,254 nm,毛蕊异黄酮葡萄糖苷、芒柄花苷、9,10-二甲氧基紫檀烷-3-O-β-D-葡萄糖苷、芒柄花素、升麻素苷、升麻素和亥茅酚苷;36~60 min,296 nm,麦冬甲基黄烷酮A和甲基麦冬二氢高异黄酮B）,进样量10 μL。以升麻素为内参物,建立其他8个指标成分的相对校正因子（RCF）,并计算各成分含量。采用外标法（ESM）测定屏风生脉胶囊中9个指标成分含量对QAMS计算结果的准确性进行验证。结果 测定了3个厂家12批屏风生脉胶囊中9个指标成分的含量,9个指标成分分别在2.68~67.00（r=0.999 4）、1.76~44.00（r=0.999 1）、2.15~53.75（r=0.999 2）、4.37~109.25（r=0.999 7）、6.58~164.50（r=0.999 5）、2.49~62.25（r=0.999 2）、1.88~47.00（r=0.999 8）、1.36~34.00（r=0.999 2）、1.09~27.25 μg·mL^–1（r=0.999 3）有良好的线性关系。平均加样回收率及RSD分别为99.34%（1.40%）、97.25%（1.13%）、98.73%（1.33%）、100.09%（0.68%）、100.04%（0.77%）、98.46%（1.26%）、97.94%（1.06%）、96.89%（1.03%）和98.90%（0.72%）。QAMS与ESM所测结果差异无统计学意义。结论 该方法操作便捷、结果准确,可用于屏风生脉胶囊中9个指标成分含量的同时测定,实现多指标质量控制。     

In vitro coronary flow after transcatheter aortic valve-in-valve implantation: A comparison of 2 valves

Background

Transcatheter aortic valve-in-valve implantation (TAVI-ViV) is an evolving treatment strategy for degenerated surgical aortic valve bioprostheses (SAVBs). However, there is some concern regarding coronary obstruction, especially after TAVI-ViV in calcified SAVBs with externally mounted leaflets. We investigated in vitro coronary flow and hydrodynamics after TAVI-ViV using 2 modern SAVBs with externally and internally mounted leaflets.